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_7705343
_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         'C19 H12 Cu N O4 S2, C3 H7 N O'
_chemical_formula_sum            'C22 H19 Cu N2 O5 S2'
_chemical_formula_weight         519.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 111.435(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.3747(7)
_cell_length_b                   13.9313(3)
_cell_length_c                   18.9465(7)
_cell_measurement_reflns_used    18962
_cell_measurement_temperature    293
_cell_measurement_theta_max      31.2490
_cell_measurement_theta_min      1.8440
_cell_volume                     5988.7(3)
_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 (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      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.910
_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    -93.00 -64.00   0.50   67.87    --  -13.20  45.00  90.00   58
  2  \w    -50.00  54.00   0.50   67.87    --  -13.20  45.00  90.00  208
  3  \w   -102.00 -76.00   0.50   67.87    --  -13.20  45.00  30.00   52
  4  \w    -52.00  -4.00   0.50   67.87    --  -13.20  45.00  30.00   96
  5  \w     26.00  52.00   0.50   67.87    --  -13.20  45.00  30.00   52
  6  \w   -102.00  76.00   0.50   67.87    --  -13.20  45.00 120.00  356
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0005458000
_diffrn_orient_matrix_UB_12      0.0444335000
_diffrn_orient_matrix_UB_13      -0.0180109000
_diffrn_orient_matrix_UB_21      0.0163800000
_diffrn_orient_matrix_UB_22      -0.0216201000
_diffrn_orient_matrix_UB_23      -0.0199598000
_diffrn_orient_matrix_UB_31      -0.0266208000
_diffrn_orient_matrix_UB_32      -0.0121940000
_diffrn_orient_matrix_UB_33      -0.0299443000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35763
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.425
_diffrn_reflns_theta_min         1.876
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52382
_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 dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         9031
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0902P)^2^+30.9259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7169
_reflns_number_total             9031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02411b2.cif
_cod_data_source_block           najh80c
_cod_depositor_comments
'Adding full bibliography for 7705341--7705344.cif.'
_cod_database_code               7705343
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Cu S2 C18 H12 O4 N'
_chemical_oxdiff_usercomment     -173
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.877
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.07
_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. Rigid bond restraints
 O1S, C2S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O1S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16), C17(H17),
 C22(H22), C23(H23), C26(H26), C27(H27), C2S(H2S)
4.b Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC)
;
_shelx_res_checksum              83618
_shelx_fab_checksum              88112
_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 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.711