The supramolecular frameworks and electrocatalytic properties of two new structurally diverse tertiary phosphane-appended nickel(ii) and copper(i) thiosquarates
Srivastava, Devyani; Kushwaha, Aparna; Kociok-Köhn, Gabriele; Gosavi, Suresh W.; Chauhan, Ratna; Kumar, Abhinav; Muddassir, Mohd.; CrystEngComm 25 (2023) 6822–6836; doi:10.1039/D3CE00817G

data_7247741
_publ_section_title
;
 The supramolecular frameworks and electrocatalytic properties of two new
 structurally diverse tertiary phosphane-appended nickel(ii) and copper(i)
 thiosquarates
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              6822
_journal_page_last               6836
_journal_paper_doi               10.1039/D3CE00817G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'C37.1 H33.25 Cl0.15 Ni O5.55 P2 S1.85, 0.06(C H2 Cl2), 0.09(C H4 O)'
_chemical_formula_sum            'C37.25 H33.73 Cl0.27 Ni O5.64 P2 S1.85'
_chemical_formula_weight         761.14
_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   mixed
_audit_creation_date             2023-10-10
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.10.06 svn.rcf4196af for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2023-11-01 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                76.6204(11)
_cell_angle_beta                 85.3079(11)
_cell_angle_gamma                81.3483(10)
_cell_formula_units_Z            2
_cell_length_a                   9.65800(14)
_cell_length_b                   10.04345(11)
_cell_length_c                   18.7630(3)
_cell_measurement_reflns_used    17838
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.6790
_cell_measurement_theta_min      4.6430
_cell_volume                     1748.37(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35359
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.868
_diffrn_reflns_theta_min         4.568
_exptl_absorpt_coefficient_mu    3.258
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             789
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6914
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0418P)^2^+1.4101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6347
_reflns_number_total             6914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00817g2.cif
_cod_data_source_block           s23gkk1a
_cod_depositor_comments
'Adding full bibliography for 7247740--7247741.cif.'
_cod_database_code               7247741
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O10-C40
 1.42 with sigma of 0.02
 Cl2-C39 \\sim Cl7-C39
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C39 \\sim Cl7 \\sim Cl2: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
O10 \\sim C40: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(Cl1) = Uanis(S1)
4. Others
 Fixed Sof: O1(0.85) O2(0.85) O3(0.85) S1(0.85) C27(0.85) C28(0.85) C29(0.85)
 C30(0.85) C31(0.85) H31A(0.85) H31B(0.85) C32(0.85) H32A(0.85) H32B(0.85)
 H32C(0.85) Cl1(0.15) Cl7(0.06) Cl2(0.06) C39(0.06) H39A(0.06) H39B(0.06)
 O10(0.09) H10A(0.09) C40(0.09) H40A(0.09) H40B(0.09) H40C(0.09)
5.a Riding coordinates:
 O10(H10A), C40(H40A,H40B,H40C)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C31(H31A,H31B), C37(H37A,H37B), C39(H39A,H39B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              71707
_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
;