#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/92/2229264.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2229264
loop_
_publ_author_name
'Kawano, Tetsuya'
'Yamane, Hisanori'
_publ_section_title
;
 Redetermination of synthetic warwickite, Mg₃TiO₂(BO₃)₂
;
_journal_coeditor_code           WM2443
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i18
_journal_page_last               i19
_journal_paper_doi               10.1107/S1600536811002157
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'Mg3 Ti O2 (B O3)2'
_chemical_formula_moiety         'B2 Mg3 O8 Ti'
_chemical_formula_structural     'Mg3 Ti O2 (B O3)2'
_chemical_formula_sum            'B2 Mg3 O8 Ti'
_chemical_formula_weight         270.45
_chemical_name_systematic
;
trimagnesium titanium(IV) dioxide bis(borate)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3013(5)
_cell_length_b                   3.10080(14)
_cell_length_c                   9.3914(6)
_cell_measurement_reflns_used    2288
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.08
_cell_volume                     270.86(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku/MSC, 2005)'
_computing_data_collection       'PROCESS-AUTO (Rigaku/MSC, 2005)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'VESTA (Momma & Izumi, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0111
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2510
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_T_max  0.839224
_exptl_absorpt_correction_T_min  0.790913
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Higashi, 1999)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.594
_refine_ls_extinction_coef       0.039(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.3981P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                348
_reflns_number_total             364
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2443.cif
_cod_data_source_block           I
_cod_database_code               2229264
_cod_database_fobs_code          2229264
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
loop_
_atom_site_type_symbol
_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
Ti Ti1 0.11388(7) 0.2500 0.07167(7) 0.0115(3) Uani d SP 0.50 . .
Mg Mg1 0.11388(7) 0.2500 0.07167(7) 0.0115(3) Uani d SP 0.50 . .
Mg Mg2 0.10160(8) 0.2500 0.68497(9) 0.0055(3) Uani d S 1 . .
B B1 0.1708(3) 0.2500 0.3719(3) 0.0061(5) Uani d S 1 . .
O O1 0.24045(19) 0.2500 0.50344(18) 0.0088(4) Uani d S 1 . .
O O2 0.25030(18) 0.2500 0.24622(19) 0.0078(4) Uani d S 1 . .
O O3 0.0255(2) 0.2500 0.36441(19) 0.0100(4) Uani d S 1 . .
O O4 0.5095(2) 0.2500 0.61439(18) 0.0100(4) Uani d S 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6.68 -1.79 -2.07 0.0883
-8.90 -2.39 -0.43 0.0867
-3.55 -0.96 2.85 0.0576
2.52 0.67 2.97 0.0350
8.37 2.25 1.13 0.0583
-1.00 -0.27 -3.08 0.0710
0.32 -9.32 -0.35 0.0988
-1.99 -6.53 2.12 0.0928
-2.47 4.23 2.64 0.0615
0.12 9.38 -0.12 0.0652
2.37 4.84 -2.53 0.0656
2.33 -5.02 -2.50 0.0900
-5.37 0.65 -2.52 0.0795
-9.30 0.04 -0.12 0.0892
2.93 -0.75 2.93 0.0377
9.19 -0.13 0.47 0.0686
6.48 0.55 -2.22 0.0823
-1.09 0.78 -3.07 0.0648
-1.43 -3.37 -2.85 0.0943
-6.64 -6.56 0.08 0.0921
1.05 3.03 2.91 0.0438
6.13 6.64 0.79 0.0332
3.57 1.64 -2.81 0.0678
5.71 -7.18 0.61 0.0783
4.00 -6.70 1.71 0.0819
-6.43 5.47 1.33 0.0750
-5.92 7.14 -0.40 0.0711
-3.56 6.46 -1.91 0.0806
6.43 -6.69 -0.39 0.0755
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 Ti1 O4 2_554 2_564 103.80(9) no
O4 Ti1 O4 2_554 6_556 83.98(6) no
O4 Ti1 O4 2_564 6_556 83.98(6) no
O4 Ti1 O2 2_554 . 101.28(6) no
O4 Ti1 O2 2_564 . 101.28(6) no
O4 Ti1 O2 6_556 . 171.31(8) no
O4 Ti1 O1 2_554 2_564 172.87(6) no
O4 Ti1 O1 2_564 2_564 82.00(5) no
O4 Ti1 O1 6_556 2_564 92.60(6) no
O2 Ti1 O1 . 2_564 81.39(6) no
O4 Ti1 O1 2_554 2_554 82.00(5) no
O4 Ti1 O1 2_564 2_554 172.87(6) no
O4 Ti1 O1 6_556 2_554 92.60(6) no
O2 Ti1 O1 . 2_554 81.39(6) no
O1 Ti1 O1 2_564 2_554 91.94(7) no
O3 Mg2 O3 5_556 5_566 101.34(9) no
O3 Mg2 O4 5_556 6_557 88.08(6) no
O3 Mg2 O4 5_566 6_557 88.08(6) no
O3 Mg2 O1 5_556 . 99.89(7) no
O3 Mg2 O1 5_566 . 99.89(7) no
O4 Mg2 O1 6_557 . 167.30(8) no
O3 Mg2 O2 5_556 2_565 175.34(6) no
O3 Mg2 O2 5_566 2_565 83.24(5) no
O4 Mg2 O2 6_557 2_565 91.24(6) no
O1 Mg2 O2 . 2_565 80.01(6) no
O3 Mg2 O2 5_556 2 83.24(5) no
O3 Mg2 O2 5_566 2 175.34(6) no
O4 Mg2 O2 6_557 2 91.24(6) no
O1 Mg2 O2 . 2 80.01(6) no
O2 Mg2 O2 2_565 2 92.17(7) no
O3 B1 O2 . . 119.1(2) yes
O3 B1 O1 . . 120.7(2) yes
O2 B1 O1 . . 120.3(2) yes
B1 O1 Mg2 . . 115.18(15) no
B1 O1 Mg1 . 2_565 123.71(9) no
Mg2 O1 Mg1 . 2_565 98.20(6) no
B1 O1 Ti1 . 2_565 123.71(9) no
Mg2 O1 Ti1 . 2_565 98.20(6) no
B1 O1 Ti1 . 2 123.71(9) no
Mg2 O1 Ti1 . 2 98.20(6) no
Mg1 O1 Ti1 2_565 2 91.94(7) no
Ti1 O1 Ti1 2_565 2 91.94(7) no
B1 O1 Mg1 . 2 123.71(9) no
Mg2 O1 Mg1 . 2 98.20(6) no
Mg1 O1 Mg1 2_565 2 91.94(7) no
Ti1 O1 Mg1 2_565 2 91.94(7) no
B1 O2 Ti1 . . 110.19(15) no
B1 O2 Mg2 . 2_564 124.49(8) no
Ti1 O2 Mg2 . 2_564 100.40(6) no
B1 O2 Mg2 . 2_554 124.49(8) no
Ti1 O2 Mg2 . 2_554 100.40(6) no
Mg2 O2 Mg2 2_564 2_554 92.17(7) no
B1 O3 Mg2 . 5_556 126.96(6) no
B1 O3 Mg2 . 5_566 126.96(6) no
Mg2 O3 Mg2 5_556 5_566 101.34(9) no
Mg1 O4 Mg1 2 2_565 103.80(9) no
Ti1 O4 Mg1 2 2_565 103.80(9) no
Mg1 O4 Ti1 2 2_565 103.80(9) no
Ti1 O4 Ti1 2 2_565 103.80(9) no
Mg1 O4 Mg1 2 6_656 96.02(6) no
Ti1 O4 Mg1 2 6_656 96.02(6) no
Mg1 O4 Mg1 2_565 6_656 96.02(6) no
Ti1 O4 Mg1 2_565 6_656 96.02(6) no
Mg1 O4 Ti1 2 6_656 96.02(6) no
Ti1 O4 Ti1 2 6_656 96.02(6) no
Mg1 O4 Ti1 2_565 6_656 96.02(6) no
Ti1 O4 Ti1 2_565 6_656 96.02(6) no
g1 O4 Mg2 2 6_657 115.24(6) no
Ti1 O4 Mg2 2 6_657 115.24(6) no
Mg1 O4 Mg2 2_565 6_657 115.24(6) no
Ti1 O4 Mg2 2_565 6_657 115.24(6) no
Mg1 O4 Mg2 6_656 6_657 126.50(10) no
Ti1 O4 Mg2 6_656 6_657 126.50(10) no
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
Ti1 O4 2_554 1.9702(12) yes
Ti1 O4 2_564 1.9702(12) yes
Ti1 O4 6_556 1.9989(19) yes
Ti1 O2 . 2.0730(18) yes
Ti1 O1 2_564 2.1565(13) yes
Ti1 O1 2_554 2.1565(13) yes
Ti1 Ti1 5 2.9502(11) no
Ti1 Mg1 5 2.9502(11) no
Ti1 Ti1 5_565 2.9502(11) no
Ti1 Mg1 5_565 2.9502(11) no
Ti1 Ti1 1_565 3.10080(14) no
Ti1 Ti1 1_545 3.10080(14) no
Mg2 O3 5_556 2.0043(12) yes
Mg2 O3 5_566 2.0043(12) yes
Mg2 O4 6_557 2.0698(19) yes
Mg2 O1 . 2.1387(19) yes
Mg2 O2 2_565 2.1522(13) yes
Mg2 O2 2 2.1522(13) yes
Mg2 Mg2 1_565 3.10080(14) no
Mg2 Mg2 1_545 3.10080(14) no
Mg2 Ti1 2_565 3.2465(9) no
Mg2 Mg1 2_565 3.2465(9) no
Mg2 Ti1 2 3.2465(9) no
Mg2 Mg1 2 3.2465(9) no
B1 O3 . 1.353(3) yes
B1 O2 . 1.393(3) yes
B1 O1 . 1.395(3) yes
