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_1564035
_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         'C30 H26 Cu N7 O2, Cl O4'
_chemical_formula_sum            'C30 H26 Cl Cu N7 O6'
_chemical_formula_weight         679.57
_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
_cell_angle_alpha                98.1050(10)
_cell_angle_beta                 111.4860(10)
_cell_angle_gamma                111.0390(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4084(4)
_cell_length_b                   12.8912(4)
_cell_length_c                   13.2892(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.84
_cell_volume                     1752.93(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27933
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.272
_diffrn_reflns_theta_min         2.407
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0731 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.9342.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8664
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0566P)^2^+1.7138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7298
_reflns_number_total             8664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           4
_cod_original_cell_volume        1752.92(10)
_cod_database_code               1564035
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C3, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, Cu1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, N7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, N7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C28 \\sim C29: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C27 \\sim C28: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C9(H9A,H9B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C3(H3), C1(H1), C19(H19), C23(H23), C7(H7), C2(H2), C22(H22),
 C18(H18), C16(H16), C11(H11), C17(H17), C15(H15), C26(H26), C13(H13), C27(H27),
  C28(H28), C30(H30), C12(H12), C14(H14), C29(H29)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2