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_7705344
_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         '0.5(C68 H48 Cu4 N12 O20 S4)'
_chemical_formula_sum            'C34 H24 Cu2 N6 O10 S2'
_chemical_formula_weight         867.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 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                90
_cell_angle_beta                 110.946(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9361(4)
_cell_length_b                   24.6960(15)
_cell_length_c                   10.4597(4)
_cell_measurement_reflns_used    13910
_cell_measurement_temperature    180
_cell_measurement_theta_max      28.9740
_cell_measurement_theta_min      2.2030
_cell_volume                     2155.77(19)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      180
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -105.00  73.00   0.50   49.01    --  -15.60  45.00 179.33  356
  2  \w   -105.00  73.00   0.50   49.01    --  -15.60  45.00 162.84  356
  3  \w   -105.00  65.00   0.50   49.01    --  -15.60  45.00 169.46  340
  4  \w    -16.00  72.00   0.50   49.01    --  -15.60  45.00  58.13  176
  5  \w   -103.00 -32.00   0.50   49.01    --  -15.60  45.00  90.00  142
  6  \w    -20.00  68.00   0.50   49.01    --  -15.60  45.00  90.00  176
  7  \w    -49.00  35.00   0.50   49.01    --  -15.60  45.00   0.00  168
  8  \w   -105.00 -64.00   0.50   49.01    --  -15.60  45.00 150.00   82
  9  \w    -12.00  18.00   0.50   49.01    --  -15.60  45.00 150.00   60
 10  \w     32.00  59.00   0.50   49.01    --  -15.60  45.00 150.00   54
 11  \w    -44.00  73.00   0.50   49.01    --  -15.60  45.00 -18.72  234
;
_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      -0.0264045000
_diffrn_orient_matrix_UB_12      0.0243941000
_diffrn_orient_matrix_UB_13      0.0209682000
_diffrn_orient_matrix_UB_21      -0.0541321000
_diffrn_orient_matrix_UB_22      -0.0149603000
_diffrn_orient_matrix_UB_23      0.0220395000
_diffrn_orient_matrix_UB_31      0.0598502000
_diffrn_orient_matrix_UB_32      -0.0027332000
_diffrn_orient_matrix_UB_33      0.0659093000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3908
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68654
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0880
_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^)+(0.1664P)^2^+3.7496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2652
_refine_ls_wR_factor_ref         0.2797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2903
_reflns_number_total             3908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02411b2.cif
_cod_data_source_block           najbc
_cod_depositor_comments
'Adding full bibliography for 7705341--7705344.cif.'
_cod_database_code               7705344
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C38 N2 Cu2 O8 S4 '
_chemical_oxdiff_usercomment     'm 90 C'
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.847
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.689(8)
 0.311(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C3-O2
 1.2 with sigma of 0.02
4. Rigid bond restraints
 O1, O102, C103
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O101
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O101, O102, C103, C4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, C9, C5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2, C4, C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O101, O102, C103
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C7: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
Uanis(O2S) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C6A)
\\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C9A) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O101) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C6) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C5) = Uanis(C6)
Uanis(C103) = Uanis(O102) = Uanis(O101)
Uanis(O1) = Uanis(C3) = Uanis(O2)
6. Rigid body (RIGU) restrains
 O1, O2, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: S8(0.5) S110(0.5) O1(0.5) O2(0.5) O101(0.5) O102(0.5) C3(0.5)
 C6(0.5) H6(0.5) C7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5) C4(0.5) C5(0.5)
 H5(0.5) C103(0.5) C4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5) C7A(0.5)
 C8A(0.5) H8A(0.5) C9A(0.5) H9A(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C5(H5), C12(H12), C13(H13), C15(H15), C16(H16),
 C18(H18), C19(H19), C21(H21), C22(H22), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A)
8.b Fitted hexagon refined as free rotating group:
 C6(C7,C8,C9,C4,C5), C4A(C5A,C6A,C7A,C8A,C9A)
;
_shelx_res_checksum              46916
_shelx_fab_checksum              34799
_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 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.756