A new Cd based metal‒organic framework for quick and convenient detection of trace water in isopropanol and 1,4-dioxane
Cheng, Feng; Fu, Ruibiao; Wen, Yuehong; Yang, Yu-Ying; Zeng, Chen; Zhang, Yuxiao; Hu, Shengmin; Wu, Xintao; Journal of Materials Chemistry C 6 (2018) 12341–; doi:10.1039/C8TC04483J

data_7237518
_publ_section_title
;
 A new Cd based metal--organic framework for quick and convenient
 detection of trace water in isopropanol and 1,4-dioxane
;
_journal_issue                   45
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              12341
_journal_paper_doi               10.1039/C8TC04483J
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C32 H28 Cd N2 O8 S2'
_chemical_formula_sum            'C32 H28 Cd N2 O8 S2'
_chemical_formula_weight         745.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-08 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                83.324(5)
_cell_angle_beta                 75.939(6)
_cell_angle_gamma                76.993(5)
_cell_formula_units_Z            1
_cell_length_a                   7.1223(5)
_cell_length_b                   7.6686(5)
_cell_length_c                   14.1045(9)
_cell_measurement_reflns_used    4226
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1470
_cell_measurement_theta_min      3.0610
_cell_volume                     726.56(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.924
_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   -115.00  65.00   0.50    5.00    --  -25.00  45.00   0.00  360
  2  \w   -115.00  25.00   0.50    5.00    --  -25.00  45.00  90.00  280
  3  \w   -115.00 -35.00   0.50    5.00    --  -25.00  45.00 180.00  160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0245710000
_diffrn_orient_matrix_UB_12      0.0197270000
_diffrn_orient_matrix_UB_13      0.0499794000
_diffrn_orient_matrix_UB_21      -0.0229943000
_diffrn_orient_matrix_UB_22      0.0928538000
_diffrn_orient_matrix_UB_23      -0.0138672000
_diffrn_orient_matrix_UB_31      -0.0992787000
_diffrn_orient_matrix_UB_32      -0.0059180000
_diffrn_orient_matrix_UB_33      0.0031016000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0057
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9710
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.096
_diffrn_reflns_theta_min         2.732
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         9710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0520
_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^)+(0.1342P)^2^+0.1289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9315
_reflns_number_total             9710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc04483j2.cif
_cod_data_source_block           cf-2_twin1_hklf4
_cod_database_code               7237518
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.7461
_shelx_estimated_absorpt_t_min   0.6589
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6923(12)
 0.3077(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Rotating group:
 O4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C2(H2), C12(H12), C10(H10), C7(H7), C3(H3), C8(H8),
 C1(H1), C11(H11), C5(H5), C13(H13)
;
_shelx_res_checksum              29295
_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 2.193
_oxdiff_exptl_absorpt_empirical_full_min 0.469
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.7445\% 
 around [0.88 0.21 0.43] (reciprocal) or [1.00 -0.00 0.00] (direct)
;