Dynamic porous coordination polymers built-up from flexible 4,4'-dithiodibenzoate and rigid N-based ligands.
Jarrah, Najmeh; Troyano, Javier; Carné-Sánchez, Arnau; Imaz, Inhar; Tangestaninejad, Shahram; Moghadam, Majid; Maspoch, Daniel; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13142–13151; doi:10.1039/d0dt02411b

data_7705342
_publ_section_title
;
 Dynamic porous coordination polymers built-up from flexible
 4,4'-dithiodibenzoate and rigid N-based ligands.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13142
_journal_page_last               13151
_journal_paper_doi               10.1039/d0dt02411b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'0.33(C114 H78 Cu6 N6 O24 S12), 0.33(C3 H7 N O)'
_chemical_formula_sum            'C39 H28.33 Cu2 N2.33 O8.33 S4'
_chemical_formula_weight         918.29
_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     iterative
_audit_creation_date             2020-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-25 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                115.86(5)
_cell_angle_beta                 103.91(5)
_cell_angle_gamma                93.65(5)
_cell_formula_units_Z            3
_cell_length_a                   10.390(6)
_cell_length_b                   21.680(6)
_cell_length_c                   21.910(6)
_cell_measurement_reflns_used    1241
_cell_measurement_temperature    100
_cell_measurement_theta_max      30
_cell_measurement_theta_min      1
_cell_volume                     4230(4)
_computing_cell_refinement       'xds (Kabsch et al., 2010)'
_computing_data_collection       'Mxcube (Gabadinho et al. 2010)'
_computing_data_reduction        'xds (Kabsch et al., 2010)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.753
_diffrn_measurement_device_type  'Pilatus DECTRIS 6M'
_diffrn_measurement_method       'w/ scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82643
_diffrn_reflns_av_R_equivalents  0.1310
_diffrn_reflns_av_unetI/netI     0.1583
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.753
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38580
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.753
_diffrn_reflns_theta_full        29.726
_diffrn_reflns_theta_max         33.813
_diffrn_reflns_theta_min         1.237
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             1402
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.729
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         16297
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.0974
_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^)+(0.1638P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2670
_refine_ls_wR_factor_ref         0.3117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7028
_reflns_number_total             16297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02411b2.cif
_cod_data_source_block           import02
_cod_depositor_comments
'Adding full bibliography for 7705341--7705344.cif.'
_cod_original_cell_volume        4230(3)
_cod_database_code               7705342
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C84-C83
 1.395 with sigma of 0.02
 C37-C36
 1.395 with sigma of 0.02
 O1S-C2S
 1.215 with sigma of 0.02
 C36-C37
 1.395 with sigma of 0.02
3. Rigid bond restraints
 C82, C83, C84
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C73, C74, C75
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N71, C72, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N81, C82, C83, C84, C85, C86
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: O1S(0.5) N3S(0.5) C2S(0.5) H2S(0.5) C5S(0.5) H5SA(0.5) H5SB(0.5)
 H5SC(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5)
6.a Me refined with riding coordinates:
 C6S(H6SA,H6SB,H6SC)
6.b Aromatic/amide H refined with riding coordinates:
 C2S(H2S), C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16),
 C17(H17), C25(H25), C26(H26), C28(H28), C29(H29), C33(H33), C34(H34), C36(H36),
  C37(H37), C45(H45), C46(H46), C48(H48), C49(H49), C53(H53), C54(H54),
 C56(H56), C57(H57), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76), C82(H82), C83(H83), C84(H84),
 C85(H85), C86(H86)
6.c Idealised Me refined as rotating group:
 C5S(H5SA,H5SB,H5SC)
;
_shelx_res_checksum              823
_shelx_fab_checksum              63095
_olex2_submission_special_instructions 'No special instructions were received'