Crystal structure of bis(μ2-1-pyrenecarboxylato-κ3 O,O′:O′)-bis(1-pyrenecarboxylato-κ2 O,O′)-(benzimidazole-κ1 N)dicadmium(II), C82H48Cd2N4O8
Gao, Peng-Fu; Li, Ting; Fu, Hong-Ru; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 377–379; doi:10.1515/ncrs-2022-0557

data_8107446
_publ_section_title
;
 Crystal structure of bis(\m2-1-pyrenecarboxylato-\k3
 O,O&#x2032;:O&#x2032;)-bis(1-pyrenecarboxylato-\k2
 O,O&#x2032;)-(benzimidazole-\k1 N)dicadmium(II), C82H48Cd2N4O8
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              377
_journal_page_last               379
_journal_paper_doi               10.1515/ncrs-2022-0557
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C82 H48 Cd2 N4 O8'
_chemical_formula_sum            'C82 H48 Cd2 N4 O8'
_chemical_formula_weight         1442.04
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                98.967(3)
_cell_angle_beta                 99.207(3)
_cell_angle_gamma                95.921(3)
_cell_formula_units_Z            1
_cell_length_a                   7.6031(3)
_cell_length_b                   10.6963(3)
_cell_length_c                   19.0717(7)
_cell_measurement_reflns_used    5385
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2620
_cell_measurement_theta_min      3.7310
_cell_volume                     1499.21(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.800
_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    -39.00 -11.00   1.00    8.00    --  -12.53  77.00   0.00   28
  2  \w     -4.00  23.00   1.00    8.00    --  -12.53 -99.00 120.00   27
  3  \w     18.00  53.00   1.00    8.00    --  -12.53  77.00   0.00   35
  4  \w    -80.00  14.00   1.00    8.00    --  -12.53 -77.00-120.00   94
  5  \w    -54.00  25.00   1.00    8.00    --   13.55 -57.00 120.00   79
  6  \w     -3.00  25.00   1.00    8.00    --   13.55  57.00 150.00   28
  7  \w     35.00  86.00   1.00    8.00    --   13.55 178.00 120.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0030935000
_diffrn_orient_matrix_UB_12      0.0141229000
_diffrn_orient_matrix_UB_13      -0.0352669000
_diffrn_orient_matrix_UB_21      -0.0845078000
_diffrn_orient_matrix_UB_22      0.0219888000
_diffrn_orient_matrix_UB_23      0.0012671000
_diffrn_orient_matrix_UB_31      0.0440183000
_diffrn_orient_matrix_UB_32      0.0624743000
_diffrn_orient_matrix_UB_33      0.0148090000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.800
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10761
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.800
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.045
_diffrn_reflns_theta_min         3.280
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5819
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.1544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4859
_reflns_number_total             7270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0557_suppl.cif
_cod_data_source_block           1
_cod_database_code               8107446
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.873
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C21(H21), C11(H11), C20(H20), C10(H10), C31(H31), C27(H27), C41(H41),
 C13(H13), C1(H1), C30(H30), C6(H6), C28(H28), C35(H35), C33(H33), C14(H14),
 C37(H37), C18(H18), C16(H16), C34(H34), C17(H17), C5(H5), C3(H3), C4(H4)
;
_shelx_res_checksum              31523
_shelx_hkl_checksum              90534
_olex2_date_sample_data_collection 2018-10-21
_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 1.672
_oxdiff_exptl_absorpt_empirical_full_min 0.704