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_7705341
_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         'C17 H15 Cu N O5 S2, 0.5(C3 H7 N O)'
_chemical_formula_sum            'C18.5 H18.5 Cu N1.5 O5.5 S2'
_chemical_formula_weight         477.51
_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
_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                102.901(5)
_cell_angle_beta                 100.793(5)
_cell_angle_gamma                113.618(5)
_cell_formula_units_Z            2
_cell_length_a                   9.960(5)
_cell_length_b                   10.210(5)
_cell_length_c                   12.060(5)
_cell_measurement_reflns_used    2981
_cell_measurement_temperature    100
_cell_measurement_theta_max      30
_cell_measurement_theta_min      1
_cell_volume                     1041.4(9)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.891
_diffrn_measured_fraction_theta_max 0.752
_diffrn_measurement_device_type  'Pilatus DECTRIS 6M'
_diffrn_measurement_method       'w/ scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.891
_diffrn_reflns_Laue_measured_fraction_max 0.752
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3976
_diffrn_reflns_point_group_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.752
_diffrn_reflns_theta_full        29.730
_diffrn_reflns_theta_max         33.846
_diffrn_reflns_theta_min         2.684
_exptl_absorpt_coefficient_mu    1.931
_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    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.682
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3976
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1597P)^2^+0.2243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2146
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3477
_reflns_number_total             3976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02411b2.cif
_cod_data_source_block           import01_tw
_cod_depositor_comments
'Adding full bibliography for 7705341--7705344.cif.'
_cod_original_cell_volume        1041.4(8)
_cod_original_formula_sum        'C18.50 H18.50 Cu N1.50 O5.50 S2'
_cod_database_code               7705341
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.744
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.543(5)
 0.457(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C12S-H12S
 1.08 with sigma of 0.02
4. Others
 Fixed Sof: O11S(0.5) N13S(0.5) C12S(0.5) H12S(0.5) C14S(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C15S(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
5.a Free rotating group:
 O11S(N13S,C12S,C14S,C15S)
5.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), C12S(H12S)
5.c Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC), C14S(H14A,H14B,H14C), C15S(H15A,
 H15B,H15C)
;
_shelx_res_checksum              93161
_olex2_submission_special_instructions 'No special instructions were received'