#------------------------------------------------------------------------------
#$Date: 2019-11-24 06:02:49 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236893 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/98/4349853.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4349853
loop_
_publ_author_name
'Gorelova, Liudmila A.'
'Pakhomova, Anna S.'
'Aprilis, Georgios'
'Dubrovinsky, Leonid S.'
'Krivovichev, Sergey V.'
_publ_section_title
;
 Pentacoordinated silicon in the high-pressure modification of datolite,
 CaBSiO4(OH)
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1653
_journal_paper_doi               10.1039/C8QI00257F
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'B Ca H O5 Si'
_chemical_formula_weight         159.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-21 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.900(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.4367(19)
_cell_length_b                   7.2074(7)
_cell_length_c                   9.2808(5)
_cell_measurement_reflns_used    1359
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      17.389
_cell_measurement_theta_min      1.502
_cell_volume                     296.74(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.517
_diffrn_measured_fraction_theta_max 0.290
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_radiation_wavelength     0.2984
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.517
_diffrn_reflns_Laue_measured_fraction_max 0.290
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            1359
_diffrn_reflns_point_group_measured_fraction_full 0.517
_diffrn_reflns_point_group_measured_fraction_max 0.290
_diffrn_reflns_theta_full        10.314
_diffrn_reflns_theta_max         17.389
_diffrn_reflns_theta_min         1.502
_exptl_absorpt_coefficient_mu    1.219
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.581
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       isosymmetrical
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.833
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         724
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2347
_refine_ls_wR_factor_ref         0.2645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                577
_reflns_number_total             724
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8qi00257f2.cif
_cod_data_source_block           shelx_CCDC7
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349853
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ca1 Ca 0.0078(4) 0.60982(10) 0.17074(9) 0.0077(7) Uani 1 1 d . .
Si1 Si 0.4897(6) 0.28081(16) 0.08052(13) 0.0063(8) Uani 1 1 d . .
B1 B 0.588(2) 0.0838(5) -0.1561(6) 0.0064(7) Uiso 1 1 d . .
O1 O 0.2508(15) 0.4241(4) 0.0294(4) 0.0092(9) Uani 1 1 d . .
O2 O 0.7108(16) 0.1910(5) -0.0352(4) 0.0092(9) Uani 1 1 d . .
O3 O 0.7086(15) 0.3407(5) 0.2138(4) 0.0092(9) Uani 1 1 d . .
O4 O 0.3019(18) 0.1033(4) 0.1392(4) 0.0092(9) Uani 1 1 d . .
O5 O 0.2602(16) 0.0919(4) -0.1597(4) 0.0092(9) Uani 1 1 d D .
H H 0.17(2) 0.052(9) -0.080(6) 0.010 Uiso 1 1 d D U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1611 0.1926 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Ca1 O1 71.1(3) . 3_565
O1 Ca1 O4 140.74(14) . 2
O1 Ca1 O4 110.2(2) 3_565 2
O1 Ca1 O2 77.0(2) . 3_665
O1 Ca1 O2 83.49(19) 3_565 3_665
O4 Ca1 O2 141.91(14) 2 3_665
O1 Ca1 O3 116.6(2) . 2_655
O1 Ca1 O3 137.97(14) 3_565 2_655
O4 Ca1 O3 89.23(17) 2 2_655
O2 Ca1 O3 60.77(14) 3_665 2_655
O1 Ca1 O3 83.28(18) . 1_455
O1 Ca1 O3 76.40(15) 3_565 1_455
O4 Ca1 O3 60.30(15) 2 1_455
O2 Ca1 O3 155.48(12) 3_665 1_455
O3 Ca1 O3 143.01(8) 2_655 1_455
O1 Ca1 O5 78.02(14) . 4_566
O1 Ca1 O5 136.24(12) 3_565 4_566
O4 Ca1 O5 76.04(19) 2 4_566
O2 Ca1 O5 119.1(2) 3_665 4_566
O3 Ca1 O5 83.60(14) 2_655 4_566
O3 Ca1 O5 69.75(18) 1_455 4_566
O1 Ca1 O5 139.28(13) . 3_565
O1 Ca1 O5 79.33(14) 3_565 3_565
O4 Ca1 O5 75.54(16) 2 3_565
O2 Ca1 O5 72.3(2) 3_665 3_565
O3 Ca1 O5 69.69(18) 2_655 3_565
O3 Ca1 O5 116.6(2) 1_455 3_565
O5 Ca1 O5 140.86(9) 4_566 3_565
O1 Ca1 B1 111.99(17) . 4_466
O1 Ca1 B1 94.9(2) 3_565 4_466
O4 Ca1 B1 30.09(14) 2 4_466
O2 Ca1 B1 169.9(2) 3_665 4_466
O3 Ca1 B1 116.30(16) 2_655 4_466
O3 Ca1 B1 30.27(14) 1_455 4_466
O5 Ca1 B1 68.7(2) 4_566 4_466
O5 Ca1 B1 97.6(2) 3_565 4_466
O1 Ca1 B1 97.4(2) . 3_665
O1 Ca1 B1 111.68(16) 3_565 3_665
O4 Ca1 B1 116.48(17) 2 3_665
O2 Ca1 B1 30.64(14) 3_665 3_665
O3 Ca1 B1 30.13(16) 2_655 3_665
O3 Ca1 B1 171.72(14) 1_455 3_665
O5 Ca1 B1 102.26(19) 4_566 3_665
O5 Ca1 B1 68.0(2) 3_565 3_665
B1 Ca1 B1 145.63(12) 4_466 3_665
O1 Ca1 Si1 93.06(12) . 3_565
O1 Ca1 Si1 23.52(12) 3_565 3_565
O4 Ca1 Si1 98.60(17) 2 3_565
O2 Ca1 Si1 79.95(13) 3_665 3_565
O3 Ca1 Si1 120.41(10) 2_655 3_565
O3 Ca1 Si1 86.82(11) 1_455 3_565
O5 Ca1 Si1 155.62(13) 4_566 3_565
O5 Ca1 Si1 55.99(9) 3_565 3_565
B1 Ca1 Si1 94.58(15) 4_466 3_565
B1 Ca1 Si1 101.36(11) 3_665 3_565
O1 Ca1 Si1 22.64(10) . .
O1 Ca1 Si1 92.15(15) 3_565 .
O4 Ca1 Si1 125.97(10) 2 .
O2 Ca1 Si1 87.15(15) 3_665 .
O3 Ca1 Si1 106.33(16) 2_655 .
O3 Ca1 Si1 79.82(14) 1_455 .
O5 Ca1 Si1 55.71(13) 4_566 .
O5 Ca1 Si1 158.46(15) 3_565 .
B1 Ca1 Si1 102.88(13) 4_466 .
B1 Ca1 Si1 97.66(17) 3_665 .
Si1 Ca1 Si1 114.98(5) 3_565 .
O1 Si1 O2 119.2(2) . .
O1 Si1 O3 117.1(2) . .
O2 Si1 O3 104.7(3) . .
O1 Si1 O4 106.0(3) . .
O2 Si1 O4 103.2(3) . .
O3 Si1 O4 105.0(2) . .
O1 Si1 Ca1 34.18(12) . 3_565
O2 Si1 Ca1 91.90(16) . 3_565
O3 Si1 Ca1 150.17(14) . 3_565
O4 Si1 Ca1 94.87(19) . 3_565
O1 Si1 Ca1 32.67(16) . .
O2 Si1 Ca1 149.76(13) . .
O3 Si1 Ca1 89.88(19) . .
O4 Si1 Ca1 98.2(3) . .
Ca1 Si1 Ca1 65.02(5) 3_565 .
O1 Si1 Ca1 95.1(2) . 3_665
O2 Si1 Ca1 37.48(16) . 3_665
O3 Si1 Ca1 94.1(2) . 3_665
O4 Si1 Ca1 140.3(2) . 3_665
Ca1 Si1 Ca1 84.05(4) 3_565 3_665
Ca1 Si1 Ca1 116.60(5) . 3_665
O1 Si1 Ca1 93.85(19) . 1_655
O2 Si1 Ca1 91.6(2) . 1_655
O3 Si1 Ca1 39.68(16) . 1_655
O4 Si1 Ca1 144.58(14) . 1_655
Ca1 Si1 Ca1 116.89(5) 3_565 1_655
Ca1 Si1 Ca1 82.81(4) . 1_655
Ca1 Si1 Ca1 63.37(5) 3_665 1_655
O1 Si1 Ca1 152.16(14) . 2_645
O2 Si1 Ca1 84.66(16) . 2_645
O3 Si1 Ca1 37.08(13) . 2_645
O4 Si1 Ca1 79.7(2) . 2_645
Ca1 Si1 Ca1 172.72(4) 3_565 2_645
Ca1 Si1 Ca1 120.34(5) . 2_645
Ca1 Si1 Ca1 96.96(9) 3_665 2_645
Ca1 Si1 Ca1 69.71(4) 1_655 2_645
O1 Si1 Ca1 90.1(2) . 2_545
O2 Si1 Ca1 135.20(16) . 2_545
O3 Si1 Ca1 88.1(2) . 2_545
O4 Si1 Ca1 32.55(19) . 2_545
Ca1 Si1 Ca1 97.54(9) 3_565 2_545
Ca1 Si1 Ca1 70.35(5) . 2_545
Ca1 Si1 Ca1 172.68(5) 3_665 2_545
Ca1 Si1 Ca1 121.49(5) 1_655 2_545
Ca1 Si1 Ca1 80.58(4) 2_645 2_545
O3 B1 O4 108.3(6) 4_565 3_655
O3 B1 O5 110.6(5) 4_565 .
O4 B1 O5 112.2(5) 3_655 .
O3 B1 O2 107.8(5) 4_565 .
O4 B1 O2 106.8(4) 3_655 .
O5 B1 O2 111.0(6) . .
O3 B1 Ca1 56.9(3) 4_565 4_665
O4 B1 Ca1 51.6(4) 3_655 4_665
O5 B1 Ca1 132.0(3) . 4_665
O2 B1 Ca1 116.9(6) . 4_665
O3 B1 Ca1 54.7(3) 4_565 3_665
O4 B1 Ca1 121.1(6) 3_655 3_665
O5 B1 Ca1 126.7(3) . 3_665
O2 B1 Ca1 53.1(3) . 3_665
Ca1 B1 Ca1 86.2(3) 4_665 3_665
Si1 O1 Ca1 124.7(2) . .
Si1 O1 Ca1 122.3(2) . 3_565
Ca1 O1 Ca1 108.9(3) . 3_565
B1 O2 Si1 120.2(6) . .
B1 O2 Ca1 96.3(4) . 3_665
Si1 O2 Ca1 117.34(19) . 3_665
B1 O3 Si1 121.0(6) 4_566 .
B1 O3 Ca1 95.1(3) 4_566 2_645
Si1 O3 Ca1 118.22(18) . 2_645
B1 O3 Ca1 92.8(3) 4_566 1_655
Si1 O3 Ca1 114.66(18) . 1_655
Ca1 O3 Ca1 111.0(2) 2_645 1_655
B1 O4 Si1 126.7(7) 3_655 .
B1 O4 Ca1 98.3(4) 3_655 2_545
Si1 O4 Ca1 124.6(2) . 2_545
B1 O5 Ca1 116.5(3) . 4_565
B1 O5 Ca1 121.2(3) . 3_565
Ca1 O5 Ca1 106.3(2) 4_565 3_565
B1 O5 H 116(6) . .
Ca1 O5 H 98(6) 4_565 .
Ca1 O5 H 95(5) 3_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.172(5) .
Ca1 O1 2.181(4) 3_565
Ca1 O4 2.253(7) 2
Ca1 O2 2.292(6) 3_665
Ca1 O3 2.336(4) 2_655
Ca1 O3 2.388(5) 1_455
Ca1 O5 2.406(4) 4_566
Ca1 O5 2.458(5) 3_565
Ca1 B1 2.846(8) 4_466
Ca1 B1 2.850(7) 3_665
Ca1 Si1 3.282(2) 3_565
Ca1 Si1 3.309(3) .
Si1 O1 1.549(5) .
Si1 O2 1.602(7) .
Si1 O3 1.619(4) .
Si1 O4 1.626(6) .
Si1 Ca1 3.282(2) 3_565
Si1 Ca1 3.346(3) 3_665
Si1 Ca1 3.398(2) 1_655
Si1 Ca1 3.414(2) 2_645
Si1 Ca1 3.447(3) 2_545
B1 O3 1.436(9) 4_565
B1 O4 1.442(6) 3_655
B1 O5 1.454(12) .
B1 O2 1.461(6) .
B1 Ca1 2.846(8) 4_665
B1 Ca1 2.850(7) 3_665
O1 Ca1 2.181(4) 3_565
O2 Ca1 2.292(6) 3_665
O3 B1 1.436(9) 4_566
O3 Ca1 2.336(4) 2_645
O3 Ca1 2.388(5) 1_655
O4 B1 1.442(6) 3_655
O4 Ca1 2.253(7) 2_545
O5 Ca1 2.406(4) 4_565
O5 Ca1 2.458(5) 3_565
O5 H 0.89(2) .
