#------------------------------------------------------------------------------
#$Date: 2024-05-05 04:51:00 +0200 (Sun 05 de May de 2024) $
#$Revision: 291626 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/55/7715512.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_7715512
loop_
_publ_author_name
'Chi, Yang'
'Xin, Mei-Ling'
_publ_section_title
;
 Chromium iodate: the structure and origin of optical second harmonic
 generation.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7093
_journal_page_last               7099
_journal_paper_doi               10.1039/d4dt00470a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Cr1 I3 O9'
_chemical_formula_sum            'Cr I3 O9'
_chemical_formula_weight         576.70
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.1319(4)
_cell_length_b                   9.1319(4)
_cell_length_c                   5.2815(3)
_cell_measurement_reflns_used    1699
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      29.74
_cell_measurement_theta_min      2.58
_cell_volume                     381.43(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4362
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.295
_diffrn_reflns_theta_min         2.575
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    13.666
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6015
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0753 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.8058.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    5.021
_exptl_crystal_description       needle
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.809
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.318
_refine_ls_abs_structure_details
;
 Flack x determined using 254 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_coef       0.0019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         843
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0326
_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)+(0.0202P)²+3.1374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.947
_reflns_Friedel_fraction_max     0.758
_reflns_number_gt                678
_reflns_number_total             843
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00470a2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7715512.cif.'
_cod_original_cell_volume        381.43(4)
_cod_database_code               7715512
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.685
_olex2_refinement_description
;
;
_shelx_res_file
;
TITL a_b.res in P6(3)
    a.res
    created by SHELXL-2018/3 at 10:10:12 on 16-Jan-2024
REM Old TITL a_a.res in P6(3)/m
REM SHELXT solution in P6(3): R1 0.120, Rweak 0.008, Alpha 0.035
REM <I/s> 2.098 for 3 systematic absences, Orientation as input
REM Flack x = 0.440 ( 0.073 ) from 183 Parsons' quotients
REM Formula found by SHELXT: O8 I3
CELL 0.71073 9.1319 9.1319 5.2815 90 90 120
ZERR 2 0.0004 0.0004 0.0003 0 0 0
LATT -1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,+X,0.5+Z
SFAC Cr I O
UNIT 2 6 18

L.S. 10
PLAN  5
SIZE 0.01 0.01 0.03
TEMP 0
CONF
LIST 6
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\a.hkl">
REM </olex2.extras>

WGHT    0.020200    3.137400
EXTI    0.001943
FVAR       0.42146
I1    2    0.316236    0.336813    0.488329    11.00000    0.01509    0.01681 =
         0.01732   -0.00054   -0.00020    0.01017
CR1   1    0.666667    0.333333    0.348502    10.33333    0.01597    0.01597 =
         0.02049    0.00000    0.00000    0.00799
O1    3    0.474700    0.283103    0.582371    11.00000    0.01482    0.01791 =
         0.02371    0.00294    0.00450    0.01044
O2    3    0.166949    0.218701    0.730317    11.00000    0.03368    0.02219 =
         0.03956    0.00454    0.02045    0.01578
O3    3    0.422669    0.547693    0.638692    11.00000    0.02297    0.01515 =
         0.02663   -0.00686    0.00110    0.01262
HKLF 4




REM  a_b.res in P6(3)
REM wR2 = 0.0707, GooF = S = 1.070, Restrained GooF = 1.069 for all data
REM R1 = 0.0326 for 678 Fo > 4sig(Fo) and 0.0561 for all 843 data
REM 41 parameters refined using 1 restraints

END

WGHT      0.0202      3.1374

REM Highest difference peak  1.809,  deepest hole -1.439,  1-sigma level  0.318
Q1    1   0.6667  0.3333  0.8361  10.33333  0.05    1.81
Q2    1   0.0000  0.0000  0.8378  10.33333  0.05    1.69
Q3    1   0.3604  0.3198  0.4899  11.00000  0.05    1.58
Q4    1   0.0000  0.0000  0.6415  10.33333  0.05    1.33
Q5    1   0.0960  0.2534  0.4902  11.00000  0.05    1.24
;
_shelx_res_checksum              95238
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.31624(7) 0.33681(7) 0.4883(4) 0.0154(2) Uani 1 1 d . . . . .
Cr1 Cr 0.666667 0.333333 0.3485(7) 0.0175(7) Uani 1 3 d S T P . .
O1 O 0.4747(10) 0.2831(10) 0.5824(15) 0.0178(17) Uani 1 1 d . . . . .
O2 O 0.1669(12) 0.2187(11) 0.730(2) 0.031(2) Uani 1 1 d . . . . .
O3 O 0.4227(11) 0.5477(10) 0.6387(19) 0.0202(17) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0151(3) 0.0168(3) 0.0173(3) -0.0005(5) -0.0002(8) 0.0102(2)
Cr1 0.0160(9) 0.0160(9) 0.0205(18) 0.000 0.000 0.0080(5)
O1 0.015(4) 0.018(4) 0.024(4) 0.003(3) 0.005(3) 0.010(3)
O2 0.034(5) 0.022(4) 0.040(6) 0.005(4) 0.020(5) 0.016(4)
O3 0.023(4) 0.015(4) 0.027(5) -0.007(3) 0.001(4) 0.013(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
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
_geom_angle_publ_flag
O1 I1 O3 95.1(4) . . ?
O2 I1 O1 96.4(4) . . ?
O2 I1 O3 99.6(4) . . ?
O1 Cr1 O1 85.9(4) 3_665 . ?
O1 Cr1 O1 85.9(4) 2_655 . ?
O1 Cr1 O1 85.9(4) 2_655 3_665 ?
O3 Cr1 O1 85.3(4) 5_554 2_655 ?
O3 Cr1 O1 170.4(4) 6_654 . ?
O3 Cr1 O1 97.3(3) 4_664 3_665 ?
O3 Cr1 O1 97.3(3) 5_554 . ?
O3 Cr1 O1 85.3(4) 4_664 . ?
O3 Cr1 O1 170.4(4) 4_664 2_655 ?
O3 Cr1 O1 97.3(3) 6_654 2_655 ?
O3 Cr1 O1 170.4(4) 5_554 3_665 ?
O3 Cr1 O1 85.3(4) 6_654 3_665 ?
O3 Cr1 O3 92.0(4) 6_654 4_664 ?
O3 Cr1 O3 92.0(4) 6_654 5_554 ?
O3 Cr1 O3 92.0(4) 5_554 4_664 ?
I1 O1 Cr1 119.7(4) . . ?
I1 O3 Cr1 131.5(5) . 4_665 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 O1 1.814(8) . ?
I1 O2 1.785(10) . ?
I1 O3 1.847(9) . ?
Cr1 O1 2.001(8) 3_665 ?
Cr1 O1 2.001(8) 2_655 ?
Cr1 O1 2.001(8) . ?
Cr1 O3 1.990(8) 5_554 ?
Cr1 O3 1.990(8) 6_654 ?
Cr1 O3 1.990(8) 4_664 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 I1 O3 Cr1 -136.0(7) . . . 4_665 ?
O2 I1 O1 Cr1 167.2(5) . . . . ?
O2 I1 O3 Cr1 -38.6(7) . . . 4_665 ?
O3 I1 O1 Cr1 -92.5(6) . . . . ?
