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###        Electronic paper (Acta Crystallographica Section E)             ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
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#            Copyright International Union of Crystallography                #
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##############################################################################
                                             
data_global
_audit_creation_method     SHELXL-97
_journal_date_recd_electronic     2002-06-28
_journal_date_accepted     2002-07-04
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2002
_journal_volume     58
_journal_issue      8
_journal_page_first     i70
_journal_page_last     i71
_journal_paper_category     EI
_publ_contact_author_name     'Dr Arthur Mar'
_publ_contact_author_address
;
Department of Chemistry
University of Alberta
Edmonton, AB
Canada T6G 2G2
;
_publ_contact_author_email     arthur.mar@ualberta.ca
_publ_contact_author_fax     '(780) 492-8231'
_publ_contact_author_phone     '(780) 492-5592'
_publ_section_title
;
Samarium orthosilicate oxyapatite, Sm₅(SiO₄)₃O
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Morgan, Mark G.'
; ?
;
; Department of Chemistry
  University of Alberta
  Edmonton, AB
  Canada T6G 2G2
;
    'Wang, Meitian'
; ?
;
; Department of Chemistry
  University of Alberta
  Edmonton, AB
  Canada T6G 2G2
;
    'Mar, Arthur'
; ?
;
; Department of Chemistry
  University of Alberta
  Edmonton, AB
  Canada T6G 2G2
;
data_I
_chemical_name_systematic     'samarium orthosilicate oxyapatite'
_chemical_name_common     'samarium orthosilicate oxyapatite'
_chemical_formula_moiety     ?
_chemical_formula_sum     'O13 Si3 Sm5'
_chemical_formula_structural     'Sm5 (Si O4)3 O'
_chemical_formula_iupac     'Sm5 (Si O4)3 O'
_chemical_formula_weight     1044.02
_chemical_melting_point     ?
_symmetry_cell_setting     hexagonal
_symmetry_space_group_name_H-M     'P 63/m'
_symmetry_space_group_name_Hall     '-P 6c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-y, x-y, z'
    '-x+y, -x, z'
    '-x, -y, z+1/2'
    'y, -x+y, z+1/2'
    'x-y, x, z+1/2'
    '-x, -y, -z'
    'y, -x+y, -z'
    'x-y, x, -z'
    'x, y, -z-1/2'
    '-y, x-y, -z-1/2'
    '-x+y, -x, -z-1/2'
_cell_length_a     9.4959(10)
_cell_length_b     9.4959(10)
_cell_length_c     7.0361(7)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     120.00
_cell_volume     549.46(10)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     4159
_cell_measurement_theta_min     4.29
_cell_measurement_theta_max     32.53
_cell_measurement_temperature     295(2)
_exptl_crystal_description     needle
_exptl_crystal_colour     red
_exptl_crystal_size_max     0.32
_exptl_crystal_size_mid     0.02
_exptl_crystal_size_min     0.02
_exptl_crystal_density_diffrn     6.310
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     912
_exptl_absorpt_coefficient_mu     26.700
_exptl_absorpt_correction_type     numerical
_exptl_absorpt_process_details     '(SHELXTL; Sheldrick, 1997)'
_exptl_absorpt_correction_T_min     0.179
_exptl_absorpt_correction_T_max     0.643
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     295(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker Platform/SMART 1000 CCD'
_diffrn_measurement_method     'ω scans (0.2°)'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     6710
_diffrn_reflns_av_R_equivalents     0.0545
_diffrn_reflns_av_sigmaI/netI     0.0252
_diffrn_reflns_theta_min     2.48
_diffrn_reflns_theta_max     32.56
_diffrn_reflns_theta_full     32.56
_diffrn_measured_fraction_theta_max     0.999
_diffrn_measured_fraction_theta_full     0.999
_diffrn_reflns_limit_h_min     -13
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     14
_diffrn_reflns_limit_l_min     -10
_diffrn_reflns_limit_l_max     10
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     716
_reflns_number_gt     650
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0358
_refine_ls_R_factor_gt     0.0308
_refine_ls_wR_factor_gt     0.0719
_refine_ls_wR_factor_ref     0.0742
_refine_ls_goodness_of_fit_ref     1.183
_refine_ls_restrained_S_all     1.183
_refine_ls_number_reflns     716
_refine_ls_number_parameters     40
_refine_ls_number_restraints     0
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
     'calc w = 1/[σ²(Fo²)+(0.0365P)²+5.6399P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     <0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     2.745
_refine_diff_density_min     -2.726
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef     0.0015(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Si' 'Si' 0.0817 0.0704
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Sm' 'Sm' -0.1638 3.4418
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'SMART (Bruker, 1997)'
_computing_cell_refinement     'SAINT (Bruker, 2000)'
_computing_data_reduction     'SAINT'
_computing_structure_solution     'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXTL'
_computing_molecular_graphics     'ATOMS (Dowty, 1999)'
_computing_publication_material     'SHELXTL'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Sm1 0.24063(5) 0.23148(5) 0.2500 0.00555(14) Uani d S 1 . . Sm
    Sm2 0.3333 0.6667 0.00046(9) 0.00990(16) Uani d S 1 . . Sm
    Si 0.0269(3) 0.3969(3) 0.2500 0.0054(4) Uani d S 1 . . Si
    O1 0.0887(6) 0.3381(6) 0.0663(7) 0.0141(9) Uani d . 6 . . O
    O2 0.1193(8) 0.5942(8) 0.2500 0.0148(13) Uani d S 1 . . O
    O3 0.4817(8) 0.1682(8) 0.2500 0.0142(13) Uani d S 1 . . O
    O4 0.0000 0.0000 0.2500 0.014(2) Uani d S 1 . . O
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Sm1 0.0047(2) 0.0056(2) 0.0066(2) 0.00283(14) 0.000 0.000
    Sm2 0.00999(19) 0.00999(19) 0.0097(3) 0.00500(10) 0.000 0.000
    Si 0.0035(9) 0.0038(9) 0.0082(10) 0.0012(7) 0.000 0.000
    O1 0.016(2) 0.024(2) 0.009(2) 0.015(2) -0.0039(17) -0.0076(18)
    O2 0.012(3) 0.007(3) 0.027(4) 0.005(2) 0.000 0.000
    O3 0.011(3) 0.005(3) 0.021(4) -0.001(2) 0.000 0.000
    O4 0.007(3) 0.007(3) 0.029(7) 0.0034(14) 0.000 0.000
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Sm1 O4 . 2.2428(4) yes
    Sm1 O1 5 2.383(5) yes
    Sm1 O1 8 2.383(5) n
    Sm1 O2 2_665 2.421(6) yes
    Sm1 O1 . 2.497(5) yes
    Sm1 O1 10_556 2.497(5) n
    Sm1 O3 . 2.641(7) yes
    Sm1 Si . 3.126(2) no
    Sm1 Si 3 3.247(2) no
    Sm1 Sm1 3 3.8847(8) no
    Sm1 Sm1 2 3.8847(8) no
    Sm1 Sm2 4_665 4.0614(6) no
    Sm2 O3 8_565 2.428(5) n
    Sm2 O3 7_665 2.428(5) n
    Sm2 O3 9 2.428(5) yes
    Sm2 O2 3_565 2.508(5) n
    Sm2 O2 . 2.508(5) yes
    Sm2 O2 2_665 2.508(5) n
    Sm2 O1 3_565 2.846(5) n
    Sm2 O1 . 2.846(5) yes
    Sm2 O1 2_665 2.846(5) n
    Sm2 Si 3_565 3.2643(18) no
    Sm2 Si . 3.2643(18) no
    Sm2 Si 2_665 3.2643(18) no
    Si O3 2 1.611(7) yes
    Si O2 . 1.623(7) yes
    Si O1 10_556 1.629(5) n
    Si O1 . 1.629(5) yes
    Si Sm1 2 3.247(2) no
    Si Sm2 10_556 3.2643(18) no
    O1 Sm1 9 2.383(5) no
    O2 Sm1 3_565 2.421(6) no
    O2 Sm2 10_556 2.508(5) no
    O3 Si 3 1.611(7) no
    O3 Sm2 4_665 2.428(5) no
    O3 Sm2 7_665 2.428(5) no
    O4 Sm1 3 2.2428(4) no
    O4 Sm1 2 2.2428(4) no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O4 Sm1 O1 . 5 103.82(12) no
    O4 Sm1 O1 . 8 103.82(12) no
    O1 Sm1 O1 5 8 138.1(3) no
    O4 Sm1 O2 . 2_665 152.20(16) no
    O1 Sm1 O2 5 2_665 85.01(12) no
    O1 Sm1 O2 8 2_665 85.01(12) no
    O4 Sm1 O1 . . 83.41(12) no
    O1 Sm1 O1 5 . 137.46(18) no
    O1 Sm1 O1 8 . 76.71(9) no
    O2 Sm1 O1 2_665 . 72.91(18) no
    O4 Sm1 O1 . 10_556 83.41(12) no
    O1 Sm1 O1 5 10_556 76.71(9) no
    O1 Sm1 O1 8 10_556 137.46(18) no
    O2 Sm1 O1 2_665 10_556 72.91(18) no
    O1 Sm1 O1 . 10_556 62.3(2) no
    O4 Sm1 O3 . . 110.57(14) no
    O1 Sm1 O3 5 . 70.52(13) no
    O1 Sm1 O3 8 . 70.52(13) no
    O2 Sm1 O3 2_665 . 97.2(2) no
    O1 Sm1 O3 . . 146.53(12) no
    O1 Sm1 O3 10_556 . 146.53(12) no
    O3 Sm2 O3 8_565 7_665 73.13(17) no
    O3 Sm2 O3 8_565 9 73.13(17) no
    O3 Sm2 O3 7_665 9 73.13(17) no
    O3 Sm2 O2 8_565 3_565 123.4(2) no
    O3 Sm2 O2 7_665 3_565 93.63(16) no
    O3 Sm2 O2 9 3_565 155.6(2) no
    O3 Sm2 O2 8_565 . 93.63(16) no
    O3 Sm2 O2 7_665 . 155.6(2) no
    O3 Sm2 O2 9 . 123.4(2) no
    O2 Sm2 O2 3_565 . 76.39(16) no
    O3 Sm2 O2 8_565 2_665 155.6(2) no
    O3 Sm2 O2 7_665 2_665 123.4(2) no
    O3 Sm2 O2 9 2_665 93.63(16) no
    O2 Sm2 O2 3_565 2_665 76.39(16) no
    O2 Sm2 O2 . 2_665 76.39(16) no
    O3 Sm2 O1 8_565 3_565 66.38(18) no
    O3 Sm2 O1 7_665 3_565 89.92(19) no
    O3 Sm2 O1 9 3_565 139.15(16) no
    O2 Sm2 O1 3_565 3_565 58.66(17) no
    O2 Sm2 O1 . 3_565 65.84(17) no
    O2 Sm2 O1 2_665 3_565 125.99(15) no
    O3 Sm2 O1 8_565 . 89.92(19) no
    O3 Sm2 O1 7_665 . 139.15(16) no
    O3 Sm2 O1 9 . 66.38(18) no
    O2 Sm2 O1 3_565 . 125.99(15) no
    O2 Sm2 O1 . . 58.66(17) no
    O2 Sm2 O1 2_665 . 65.84(17) no
    O1 Sm2 O1 3_565 . 117.41(6) no
    O3 Sm2 O1 8_565 2_665 139.15(16) no
    O3 Sm2 O1 7_665 2_665 66.38(18) no
    O3 Sm2 O1 9 2_665 89.92(19) no
    O2 Sm2 O1 3_565 2_665 65.84(17) no
    O2 Sm2 O1 . 2_665 125.99(15) no
    O2 Sm2 O1 2_665 2_665 58.66(17) no
    O1 Sm2 O1 3_565 2_665 117.41(6) no
    O1 Sm2 O1 . 2_665 117.41(5) no
    O3 Si O2 2 . 113.1(4) no
    O3 Si O1 2 10_556 110.7(2) no
    O2 Si O1 . 10_556 108.4(2) no
    O3 Si O1 2 . 110.7(2) no
    O2 Si O1 . . 108.4(2) no
    O1 Si O1 10_556 . 105.0(4) no
    Si O1 Sm1 . 9 140.8(3) no
    Si O1 Sm1 . . 96.2(2) no
    Sm1 O1 Sm1 9 . 117.46(19) no
    Si O1 Sm2 . . 89.4(2) no
    Sm1 O1 Sm2 9 . 101.55(19) no
    Sm1 O1 Sm2 . . 102.03(16) no
    Si O2 Sm1 . 3_565 126.2(4) no
    Si O2 Sm2 . 10_556 102.3(2) no
    Sm1 O2 Sm2 3_565 10_556 115.09(19) no
    Si O2 Sm2 . . 102.3(2) no
    Sm1 O2 Sm2 3_565 . 115.09(19) no
    Sm2 O2 Sm2 10_556 . 88.9(2) no
    Si O3 Sm2 3 4_665 126.2(2) no
    Si O3 Sm2 3 7_665 126.2(2) no
    Sm2 O3 Sm2 4_665 7_665 93.1(2) no
    Si O3 Sm1 3 . 96.6(3) no
    Sm2 O3 Sm1 4_665 . 106.4(2) no
    Sm2 O3 Sm1 7_665 . 106.4(2) no
    Sm1 O4 Sm1 . 3 120.0 no
    Sm1 O4 Sm1 . 2 120.0 no
    Sm1 O4 Sm1 3 2 120.0 no
