Five-coordinate [(L2)2CuII(X)]z+ (X = H2O, z = 2; X = N3−, SCN−, NO2−, MeCO2−, Cl−, Br−, z = 1; L2 = 1-benzyl-[3-(2-pyridyl)]pyrazole) complexes: Structural index, EPR and redox potential correlations
Mukherjee, Jhumpa; Sengupta, Arunava; Mukherjee, Rabindranath; Inorganica Chimica Acta 513 (2020) 119899–; doi:10.1016/j.ica.2020.119899

data_1564036
_publ_section_title
;
 Five-coordinate [(L2)2CuII(X)]z+ (X&#x00A0;=&#x00A0;H2O,
 z&#x00A0;=&#x00A0;2; X&#x00A0;=&#x00A0;N3&#x2212;, SCN&#x2212;,
 NO2&#x2212;, MeCO2&#x2212;, Cl&#x2212;, Br&#x2212;, z&#x00A0;=&#x00A0;1;
 L2&#x00A0;=&#x00A0;1-benzyl-[3-(2-pyridyl)]pyrazole) complexes:
 Structural index, EPR and redox potential correlations
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119899
_journal_paper_doi               10.1016/j.ica.2020.119899
_journal_volume                  513
_journal_year                    2020
_chemical_formula_moiety         'C32 H29 Cu N6 O2, Cl O4, 3(H2 O)'
_chemical_formula_sum            'C32 H35 Cl Cu N6 O9'
_chemical_formula_weight         746.65
_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
_cell_angle_alpha                100.540(5)
_cell_angle_beta                 107.460(5)
_cell_angle_gamma                109.854(5)
_cell_formula_units_Z            2
_cell_length_a                   11.962(5)
_cell_length_b                   12.712(5)
_cell_length_c                   12.988(5)
_cell_measurement_reflns_used    5281
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      1.72
_cell_volume                     1680.3(12)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8834
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.733
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5845
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0634P)^2^+2.0119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5281
_reflns_number_total             5845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           5
_cod_database_code               1564036
_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,H) groups
2. Rigid bond restraints
 C28, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Free rotating group:
 O0AA(H0AA,H0AB), O1AA(H1AA,H1AB), O2AA(H2AA,H2AB)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C24(H24A,H24B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C19(H19), C7(H7), C17(H17), C16(H16), C22(H22), C1(H1), C18(H18),
 C23(H23), C15(H15), C4(H4), C2(H2), C11(H11), C3(H3), C14(H14), C26(H26),
 C13(H13), C12(H12), C30(H30), C27(H27), C28(H28), C29(H29)
3.d Idealised Me refined as rotating group:
 C014(H01A,H01B,H01C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2