#------------------------------------------------------------------------------
#$Date: 2021-07-08 10:40:26 +0300 (Thu, 08 Jul 2021) $
#$Revision: 267378 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/40/1564033.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1564033
loop_
_publ_author_name
'Mukherjee, Jhumpa'
'Sengupta, Arunava'
'Mukherjee, Rabindranath'
_publ_section_title
;
 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
;
_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 N9, Cl O4'
_chemical_formula_sum            'C30 H26 Cl Cu N9 O4'
_chemical_formula_weight         675.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 105.886(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.320(5)
_cell_length_b                   23.292(5)
_cell_length_c                   10.738(5)
_cell_measurement_reflns_used    6042
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.278
_cell_measurement_theta_min      2.16
_cell_volume                     2963.7(19)
_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 (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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19625
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.840
_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_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   28.28
_exptl_transmission_factor_min   2.16
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0395
_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/[σ²(Fo²)+(0.0555P)²+0.8730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6042
_reflns_number_total             7303
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           2
_cod_database_code               1564033
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C4(H4), C8(H8), C22(H22), C23(H23), C14(H14), C19(H19), C3(H3),
 C7(H7), C2(H2), C1(H1), C17(H17), C13(H13), C18(H18), C16(H16), C12(H12),
 C28(H28), C11(H11), C26(H26), C29(H29), C30(H30), C27(H27)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu 0.19018(2) 0.19397(2) 0.61405(2) 0.01298(8) Uani 1 1 d . . . . .
Cl Cl 0.70283(4) 0.06552(2) 0.90816(5) 0.01727(11) Uani 1 1 d . . . . .
O2 O 0.72660(13) 0.11431(6) 0.83695(17) 0.0292(4) Uani 1 1 d . . . . .
N6 N 0.44997(13) 0.17074(7) 0.64470(17) 0.0164(3) Uani 1 1 d . . . . .
O3 O 0.76426(16) 0.07150(7) 1.04187(17) 0.0397(4) Uani 1 1 d . . . . .
O4 O 0.73655(18) 0.01365(7) 0.85818(18) 0.0422(5) Uani 1 1 d . . . . .
N1 N 0.03315(13) 0.21725(7) 0.62300(16) 0.0147(3) Uani 1 1 d . . . . .
O1 O 0.58519(14) 0.06411(8) 0.8975(2) 0.0429(5) Uani 1 1 d . . . . .
N2 N 0.14152(13) 0.12248(6) 0.73686(16) 0.0143(3) Uani 1 1 d . . . . .
N3 N 0.18127(14) 0.07667(7) 0.81156(16) 0.0161(3) Uani 1 1 d . . . . .
N9 N 0.20219(16) 0.22548(7) 0.96167(17) 0.0219(4) Uani 1 1 d . . . . .
N5 N 0.33825(13) 0.16646(6) 0.58686(16) 0.0141(3) Uani 1 1 d . . . . .
N8 N 0.22700(13) 0.23310(7) 0.86599(16) 0.0155(3) Uani 1 1 d . . . . .
N4 N 0.13250(14) 0.14896(7) 0.44464(16) 0.0155(3) Uani 1 1 d . . . . .
C20 C 0.21433(17) 0.12806(8) 0.39492(19) 0.0162(4) Uani 1 1 d . . . . .
C10 C 0.26850(17) 0.01799(8) 0.6744(2) 0.0170(4) Uani 1 1 d . . . . .
C15 C 0.35885(18) 0.01137(9) 0.6212(2) 0.0226(4) Uani 1 1 d . . . . .
H15 H 0.4290 0.0267 0.6633 0.027 Uiso 1 1 calc R . . . .
C4 C -0.12144(17) 0.20287(8) 0.7148(2) 0.0179(4) Uani 1 1 d . . . . .
H4 H -0.1563 0.1808 0.7650 0.021 Uiso 1 1 calc R . . . .
C21 C 0.32868(16) 0.14062(8) 0.4729(2) 0.0157(4) Uani 1 1 d . . . . .
N7 N 0.25521(14) 0.24216(7) 0.76995(17) 0.0183(4) Uani 1 1 d . . . . .
C25 C 0.54518(17) 0.25651(9) 0.7587(2) 0.0208(4) Uani 1 1 d . . . . .
C24 C 0.49450(17) 0.19852(8) 0.7695(2) 0.0186(4) Uani 1 1 d . . . . .
H24A H 0.5517 0.1740 0.8242 0.022 Uiso 1 1 calc R . . . .
H24B H 0.4342 0.2029 0.8108 0.022 Uiso 1 1 calc R . . . .
C8 C 0.10806(18) 0.05876(9) 0.8772(2) 0.0208(4) Uani 1 1 d . . . . .
H8 H 0.1175 0.0274 0.9328 0.025 Uiso 1 1 calc R . . . .
C22 C 0.43517(17) 0.12888(8) 0.4565(2) 0.0207(4) Uani 1 1 d . . . . .
H22 H 0.4518 0.1116 0.3858 0.025 Uiso 1 1 calc R . . . .
C5 C -0.01795(16) 0.18603(8) 0.69712(19) 0.0142(4) Uani 1 1 d . . . . .
C23 C 0.50935(17) 0.14848(9) 0.5676(2) 0.0208(4) Uani 1 1 d . . . . .
H23 H 0.5876 0.1468 0.5869 0.025 Uiso 1 1 calc R . . . .
C14 C 0.3442(2) -0.01816(9) 0.5050(2) 0.0264(5) Uani 1 1 d . . . . .
H14 H 0.4048 -0.0222 0.4697 0.032 Uiso 1 1 calc R . . . .
C19 C 0.18976(19) 0.09566(9) 0.2825(2) 0.0225(4) Uani 1 1 d . . . . .
H19 H 0.2473 0.0819 0.2497 0.027 Uiso 1 1 calc R . . . .
C3 C -0.17132(17) 0.25269(9) 0.6569(2) 0.0209(4) Uani 1 1 d . . . . .
H3 H -0.2399 0.2647 0.6683 0.025 Uiso 1 1 calc R . . . .
C7 C 0.01738(17) 0.09539(8) 0.8465(2) 0.0193(4) Uani 1 1 d . . . . .
H7 H -0.0465 0.0944 0.8768 0.023 Uiso 1 1 calc R . . . .
C2 C -0.11861(17) 0.28473(9) 0.5814(2) 0.0211(4) Uani 1 1 d . . . . .
H2 H -0.1513 0.3183 0.5414 0.025 Uiso 1 1 calc R . . . .
C9 C 0.28514(16) 0.04913(8) 0.8017(2) 0.0176(4) Uani 1 1 d . . . . .
H9A H 0.3104 0.0220 0.8723 0.021 Uiso 1 1 calc R . . . .
H9B H 0.3434 0.0780 0.8101 0.021 Uiso 1 1 calc R . . . .
C6 C 0.04255(16) 0.13470(8) 0.75904(19) 0.0140(4) Uani 1 1 d . . . . .
C1 C -0.01683(17) 0.26580(8) 0.5670(2) 0.0178(4) Uani 1 1 d . . . . .
H1 H 0.0188 0.2873 0.5167 0.021 Uiso 1 1 calc R . . . .
C17 C -0.00556(19) 0.10561(9) 0.2699(2) 0.0235(4) Uani 1 1 d . . . . .
H17 H -0.0812 0.0985 0.2288 0.028 Uiso 1 1 calc R . . . .
C13 C 0.2411(2) -0.04143(9) 0.4415(2) 0.0261(5) Uani 1 1 d . . . . .
H13 H 0.2319 -0.0610 0.3639 0.031 Uiso 1 1 calc R . . . .
C18 C 0.0782(2) 0.08416(9) 0.2201(2) 0.0261(5) Uani 1 1 d . . . . .
H18 H 0.0597 0.0621 0.1450 0.031 Uiso 1 1 calc R . . . .
C16 C 0.02506(17) 0.13789(9) 0.3817(2) 0.0205(4) Uani 1 1 d . . . . .
H16 H -0.0315 0.1526 0.4147 0.025 Uiso 1 1 calc R . . . .
C12 C 0.15115(19) -0.03528(9) 0.4946(2) 0.0250(5) Uani 1 1 d . . . . .
H12 H 0.0815 -0.0512 0.4528 0.030 Uiso 1 1 calc R . . . .
C28 C 0.6442(2) 0.36269(10) 0.7543(3) 0.0381(7) Uani 1 1 d . . . . .
H28 H 0.6772 0.3985 0.7524 0.046 Uiso 1 1 calc R . . . .
C11 C 0.16444(17) -0.00561(9) 0.6094(2) 0.0210(4) Uani 1 1 d . . . . .
H11 H 0.1032 -0.0014 0.6436 0.025 Uiso 1 1 calc R . . . .
C26 C 0.5030(2) 0.29253(10) 0.6557(3) 0.0353(6) Uani 1 1 d . . . . .
H26 H 0.4413 0.2815 0.5885 0.042 Uiso 1 1 calc R . . . .
C29 C 0.6853(2) 0.32681(11) 0.8571(3) 0.0362(6) Uani 1 1 d . . . . .
H29 H 0.7459 0.3382 0.9254 0.043 Uiso 1 1 calc R . . . .
C30 C 0.63689(19) 0.27367(10) 0.8594(2) 0.0283(5) Uani 1 1 d . . . . .
H30 H 0.6657 0.2491 0.9288 0.034 Uiso 1 1 calc R . . . .
C27 C 0.5538(3) 0.34600(11) 0.6530(3) 0.0440(7) Uani 1 1 d . . . . .
H27 H 0.5267 0.3704 0.5829 0.053 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Cu N2 76.47(6) . .
N1 Cu N4 94.30(6) . .
N5 Cu N1 173.80(7) . .
N5 Cu N2 103.85(6) . .
N5 Cu N4 79.50(7) . .
N4 Cu N2 93.27(7) . .
N7 Cu N1 88.80(7) . .
N7 Cu N2 91.95(7) . .
N7 Cu N5 97.37(7) . .
N7 Cu N4 174.43(6) . .
O3 Cl O2 109.00(11) . .
O4 Cl O2 110.16(10) . .
O4 Cl O3 109.26(11) . .
O1 Cl O2 109.00(10) . .
O1 Cl O3 109.23(13) . .
O1 Cl O4 110.17(12) . .
N5 N6 C24 122.49(16) . .
C23 N6 N5 110.20(17) . .
C23 N6 C24 127.24(17) . .
C5 N1 Cu 119.03(13) . .
C1 N1 Cu 121.74(13) . .
C1 N1 C5 118.93(16) . .
N3 N2 Cu 143.73(12) . .
C6 N2 Cu 109.97(12) . .
C6 N2 N3 105.31(15) . .
N2 N3 C8 111.68(16) . .
N2 N3 C9 119.27(15) . .
C8 N3 C9 128.60(17) . .
N6 N5 Cu 138.97(13) . .
C21 N5 Cu 114.55(13) . .
C21 N5 N6 106.10(15) . .
N9 N8 N7 177.8(2) . .
C20 N4 Cu 114.77(13) . .
C16 N4 Cu 127.02(13) . .
C16 N4 C20 118.19(18) . .
N4 C20 C21 114.07(17) . .
N4 C20 C19 122.07(19) . .
C19 C20 C21 123.81(18) . .
C15 C10 C9 119.90(19) . .
C15 C10 C11 118.7(2) . .
C11 C10 C9 121.36(17) . .
C10 C15 C14 120.0(2) . .
C3 C4 C5 119.06(18) . .
N5 C21 C20 116.41(16) . .
N5 C21 C22 110.63(18) . .
C22 C21 C20 132.90(19) . .
N8 N7 Cu 118.76(13) . .
C26 C25 C24 122.5(2) . .
C26 C25 C30 119.9(2) . .
C30 C25 C24 117.6(2) . .
N6 C24 C25 112.85(17) . .
N3 C8 C7 107.34(17) . .
C23 C22 C21 104.50(18) . .
N1 C5 C4 121.21(17) . .
N1 C5 C6 116.33(17) . .
C4 C5 C6 122.44(17) . .
N6 C23 C22 108.57(18) . .
C13 C14 C15 120.9(2) . .
C18 C19 C20 118.69(19) . .
C4 C3 C2 119.62(18) . .
C8 C7 C6 104.57(17) . .
C1 C2 C3 118.68(19) . .
N3 C9 C10 111.80(16) . .
N2 C6 C5 117.89(16) . .
N2 C6 C7 111.07(16) . .
C7 C6 C5 130.96(17) . .
N1 C1 C2 122.48(18) . .
C16 C17 C18 118.7(2) . .
C14 C13 C12 119.3(2) . .
C17 C18 C19 119.5(2) . .
N4 C16 C17 122.87(19) . .
C11 C12 C13 120.4(2) . .
C29 C28 C27 120.3(2) . .
C12 C11 C10 120.75(19) . .
C25 C26 C27 119.3(3) . .
C28 C29 C30 119.8(2) . .
C29 C30 C25 120.5(2) . .
C28 C27 C26 120.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N1 2.0366(17) .
Cu N2 2.3031(16) .
Cu N5 2.0286(17) .
Cu N4 2.0507(18) .
Cu N7 1.9924(18) .
Cl O2 1.4439(15) .
Cl O3 1.4348(18) .
Cl O4 1.4292(16) .
Cl O1 1.4226(18) .
N6 N5 1.350(2) .
N6 C24 1.453(3) .
N6 C23 1.349(3) .
N1 C5 1.354(2) .
N1 C1 1.348(2) .
N2 N3 1.344(2) .
N2 C6 1.335(2) .
N3 C8 1.354(2) .
N3 C9 1.461(2) .
N9 N8 1.163(2) .
N5 C21 1.339(3) .
N8 N7 1.194(2) .
N4 C20 1.354(2) .
N4 C16 1.336(3) .
C20 C21 1.458(3) .
C20 C19 1.385(3) .
C10 C15 1.391(3) .
C10 C9 1.512(3) .
C10 C11 1.394(3) .
C15 C14 1.393(3) .
C4 C5 1.396(3) .
C4 C3 1.379(3) .
C21 C22 1.398(3) .
C25 C24 1.506(3) .
C25 C26 1.371(3) .
C25 C30 1.392(3) .
C8 C7 1.372(3) .
C22 C23 1.368(3) .
C5 C6 1.468(3) .
C14 C13 1.378(3) .
C19 C18 1.380(3) .
C3 C2 1.387(3) .
C7 C6 1.406(3) .
C2 C1 1.377(3) .
C17 C18 1.379(3) .
C17 C16 1.379(3) .
C13 C12 1.385(3) .
C12 C11 1.383(3) .
C28 C29 1.367(4) .
C28 C27 1.382(4) .
C26 C27 1.398(3) .
C29 C30 1.377(3) .
