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_2108834
_publ_section_title
;
 Crystal structure or chemical composition of salt--sugar-based
 metal--organic frameworks: what are the nonlinear optical properties due
 to?
;
_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(I), C12 H28 Ca O12'
_chemical_formula_sum            'C12 H28 Ca I2 O12'
_chemical_formula_weight         658.22
_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.r6257)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.233(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6384(3)
_cell_length_b                   14.4621(4)
_cell_length_c                   10.7490(3)
_cell_measurement_reflns_used    6384
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.8760
_cell_measurement_theta_min      4.3350
_cell_volume                     1121.14(7)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -73.00 -44.00   1.00    4.00    --  -42.64  77.00-150.00   29
  2  \w    -28.00  47.00   1.00    4.00    --   42.64 -57.00-150.00   75
  3  \w     11.00 115.00   1.00    4.00    --   42.64  77.00 -30.00  104
  4  \w    -19.00  30.00   1.00    4.00    --   42.64 -57.00  60.00   49
  5  \w     86.00 116.00   1.00   10.00    --   92.50  45.00-120.00   30
  6  \w     39.00 106.00   1.00   10.00    --   92.50 -70.00  -1.27   67
  7  \w     19.00 104.00   1.00   10.00    --   92.50 -70.00  77.61   85
  8  \w     72.00  98.00   1.00   10.00    --   92.50  45.00  90.00   26
  9  \w     70.00 122.00   1.00   10.00    --   92.50 -70.00 -92.78   52
 10  \w    110.00 136.00   1.00   10.00    --   92.50  45.00  90.00   26
 11  \w     21.00  61.00   1.00   10.00    --   92.50 -61.00 150.00   40
 12  \w     20.00 114.00   1.00   10.00    --   92.50 -70.00-157.10   94
 13  \w     16.00  60.00   1.00   10.00    --   92.50 -30.00   0.00   44
 14  \w    105.00 131.00   1.00   10.00    --   92.50  61.00-180.00   26
 15  \w     73.00  98.00   1.00   10.00    --   92.50  30.00  60.00   25
 16  \w     61.00  98.00   1.00   10.00    --   92.50 -70.00 120.55   37
 17  \w    106.00 163.00   1.00   10.00    --   92.50  45.00 -90.00   57
 18  \w    131.00 166.00   1.00   10.00    --   92.50  30.00  60.00   35
 19  \w     93.00 120.00   1.00   10.00    --   92.50  77.00 -30.00   27
 20  \w    126.00 162.00   1.00   10.00    --   92.50  45.00 -60.00   36
 21  \w     97.00 122.00   1.00   10.00    --   92.50  61.00  30.00   25
 22  \w    126.00 158.00   1.00   10.00    --   92.50  61.00  30.00   32
 23  \w     46.00  72.00   1.00   10.00    --   92.50 -61.00-120.00   26
 24  \w     74.00 109.00   1.00   10.00    --   92.50 -61.00 150.00   35
 25  \w     27.00  52.00   1.00   10.00    --   92.50 -45.00  30.00   25
 26  \w     90.00 116.00   1.00   10.00    --   92.50 -45.00  30.00   26
 27  \w     77.00 102.00   1.00   10.00    --   92.50  45.00 -90.00   25
 28  \w     96.00 121.00   1.00   10.00    --   92.50 -30.00   0.00   25
 29  \w     68.00 147.00   1.00   10.00    --   92.50  30.00  30.00   79
 30  \w     87.00 155.00   1.00   10.00    --   92.50  45.00 -30.00   68
 31  \w     37.00  63.00   1.00   10.00    --   92.50 -70.00 -92.78   26
 32  \w     96.00 122.00   1.00   10.00    --   92.50 -61.00-120.00   26
 33  \w     73.00  98.00   1.00   10.00    --   92.50 -66.00  25.21   25
 34  \w     58.00  83.00   1.00   10.00    --   92.50 -70.00-125.03   25
 35  \w     21.00  46.00   1.00   10.00    --   92.50 -67.00 -68.04   25
 36  \w     72.00  98.00   1.00   10.00    --   92.50 -70.00 -58.23   26
 37  \w     23.00  51.00   1.00   10.00    --   92.50 -70.00 -58.23   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0168014000
_diffrn_orient_matrix_UB_12      -0.0861180000
_diffrn_orient_matrix_UB_13      -0.0797024000
_diffrn_orient_matrix_UB_21      0.0906509000
_diffrn_orient_matrix_UB_22      -0.0535551000
_diffrn_orient_matrix_UB_23      0.1291305000
_diffrn_orient_matrix_UB_31      -0.1926682000
_diffrn_orient_matrix_UB_32      -0.0327776000
_diffrn_orient_matrix_UB_33      -0.0016926000
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11076
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        66.914
_diffrn_reflns_theta_max         66.914
_diffrn_reflns_theta_min         4.356
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.519
_exptl_absorpt_correction_T_max  0.337
_exptl_absorpt_correction_T_min  0.091
_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    1.950
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1525 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3737
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0436P)^2^+0.4062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.877
_reflns_Friedel_fraction_max     0.877
_reflns_number_gt                3590
_reflns_number_total             3737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            um5049sup1.cif
_cod_data_source_block           CaDgalI_new
_cod_original_cell_volume        1121.14(6)
_cod_database_code               2108834
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ca(C6H10O5)I2(H2O)2
_reflns_odcompleteness_completeness 98.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B), C3A(H3AA), C3B(H3BA), C4A(H4AA), C4B(H4BA), C5A(H5AA),
 C5B(H5BA)
2.c Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C6A(H6AA,H6AB), C6B(H6BA,H6BB)
2.d Idealised tetrahedral OH refined as rotating group:
 O2A(H2A), O2B(H2B), O3A(H3A), O3B(H3B), O4A(H4A), O4B(H4B), O5A(H5A), O5B(H5B)
;
_shelx_res_checksum              55201
_shelx_hkl_checksum              20817
_olex2_submission_original_sample_id CaDGalI
_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 1.660
_oxdiff_exptl_absorpt_empirical_full_min 0.727
_cod_database_fobs_code 2108834