Crystal structure or chemical composition of salt‒sugar-based metal‒organic frameworks: what are the nonlinear optical properties due to?
Marabello, Domenica; Antoniotti, Paola; Benzi, Paola; Beccari, Fabio; Canepa, Carlo; Cariati, Elena; Cioci, Alma; Lo Presti, Leonardo; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S2052520621004637

data_2108833
_publ_section_title
;
 Crystal structure or chemical composition of salt--sugar-based
 metal--organic frameworks: what are the nonlinear optical properties due
 to?
;
_journal_coeditor_code           UM5049SUP1
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621004637
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         '2(Br), C12 H28 Ca O12'
_chemical_formula_sum            'C12 H28 Br2 Ca O12'
_chemical_formula_weight         564.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.931(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5022(4)
_cell_length_b                   14.2259(6)
_cell_length_c                   10.4517(6)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    293
_cell_measurement_theta_max      61.2290
_cell_measurement_theta_min      6.2580
_cell_volume                     1048.65(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 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      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2890
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -27.00   5.00   1.00   10.00    --    0.00  57.00 -30.00   32
  2  \w     27.00  73.00   1.00   10.00    --    0.00  57.00 -30.00   46
  3  \w     35.00  69.00   1.00   10.00    --    0.00  37.00  90.00   34
  4  \w    -18.00  27.00   1.00   10.00    --    0.00  37.00  90.00   45
  5  \w     21.00  52.00   1.00   30.00    --   82.02 -70.00 110.46   31
  6  \w     57.00  99.00   1.00   30.00    --   82.02 -70.00 110.46   42
  7  \w      9.00  35.00   1.00   30.00    --   82.02 -70.00-122.02   26
  8  \w     45.00 164.00   1.00   30.00    --   82.02  15.00 120.00  119
  9  \w      9.00 100.00   1.00   30.00    --   82.02 -69.00 -88.33   91
 10  \w     46.00  72.00   1.00   30.00    --   82.02 -70.00 -17.65   26
 11  \w      8.00 100.00   1.00   30.00    --   82.02 -70.00  12.81   92
 12  \w     72.00  98.00   1.00   30.00    --   82.02 -70.00-122.02   26
 13  \w     72.00 110.00   1.00   30.00    --   82.02 -69.00 150.90   38
 14  \w     90.00 155.00   1.00   30.00    --   82.02  45.00 -30.00   65
 15  \w     77.00 125.00   1.00   30.00    --   82.02  45.00-150.00   48
 16  \w     18.00  43.00   1.00   30.00    --   82.02 -69.00 150.90   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0293437000
_diffrn_orient_matrix_UB_12      0.1013169000
_diffrn_orient_matrix_UB_13      -0.0408413000
_diffrn_orient_matrix_UB_21      -0.0441453000
_diffrn_orient_matrix_UB_22      -0.0321280000
_diffrn_orient_matrix_UB_23      -0.1484043000
_diffrn_orient_matrix_UB_31      -0.2119239000
_diffrn_orient_matrix_UB_32      0.0206770000
_diffrn_orient_matrix_UB_33      -0.0298109000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5021
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        58.934
_diffrn_reflns_theta_max         58.934
_diffrn_reflns_theta_min         4.500
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.561
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 913 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2698
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0350
_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/[\s^2^(Fo^2^)+(0.0283P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.786
_reflns_Friedel_fraction_max     0.786
_reflns_number_gt                2457
_reflns_number_total             2698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            um5049sup1.cif
_cod_data_source_block           CaDgalBr_new
_cod_database_code               2108833
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H27 Br2 Ca O12'
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2AA,H2AB} of C2A, {H6AA,H6AB} of C6A, {H2BA,H2BB} of C2B
 At 1.5 times of:
  All O(H) groups, {H6BA,H6BB} of C6B, All O(H,H) groups
2. Restrained distances
 O3A-H3A
 0.85 with sigma of 0.01
 O3B-H3B
 0.85 with sigma of 0.01
 O2B-H2B
 0.85 with sigma of 0.01
 H1WA-O1W
 0.85 with sigma of 0.02
 H2WB-O2W
 0.85 with sigma of 0.02
 H2WA-O2W
 0.85 with sigma of 0.02
 O4A-H4A
 0.85 with sigma of 0.01
 C3A-H3A
 1.908902 with sigma of 0.02
 Ca1-H3A
 3.106448 with sigma of 0.02
 C3B-H3B
 1.91536 with sigma of 0.02
 Ca1-H3B
 2.88019 with sigma of 0.02
 C1B-H2B
 1.895331 with sigma of 0.02
 Ca1-H2B
 3.015166 with sigma of 0.02
 H1WA-Ca1
 2.9 with sigma of 0.04
 Ca1-H4A
 3.094445 with sigma of 0.02
 C4A-H4A
 1.900765 with sigma of 0.02
3.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B), C3A(H3AA), C3B(H3BA), C4A(H4AA), C4B(H4BA), C5A(H5AA),
 C5B(H5BA)
3.c Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C6A(H6AA,H6AB), C6B(H6BA,H6BB)
3.d Idealised tetrahedral OH refined as rotating group:
 O2A(H2A), O2B(H2B), O3A(H3A), O3B(H3B), O4B(H4B), O5A(H5A), O5B(H5B)
;
_shelx_res_checksum              12475
_shelx_hkl_checksum              11740
_olex2_submission_original_sample_id CaDGalBr
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.793
_cod_database_fobs_code 2108833