Dimeric metallacycles and coordination polymers: Zn(II), Cd(II) and Hg(II) complexes of two positional isomers of a flexible N,O-hybrid bispyrazole derived ligand
Soldevila-Sanmartín, Joan; Guerrero, Miguel; Choquesillo-Lazarte, Duane; Giner Planas, José; Pons, Josefina; Inorganica Chimica Acta 506 (2020) 119549–; doi:10.1016/j.ica.2020.119549

data_1565161
_publ_section_title
;
 Dimeric metallacycles and coordination polymers: Zn(II), Cd(II) and
 Hg(II) complexes of two positional isomers of a flexible N,O-hybrid
 bispyrazole derived ligand
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119549
_journal_paper_doi               10.1016/j.ica.2020.119549
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         'C44 H60 Cd2 Cl4 N8 O4'
_chemical_formula_sum            'C44 H60 Cd2 Cl4 N8 O4'
_chemical_formula_weight         1131.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 97.179(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5328(8)
_cell_length_b                   19.3000(16)
_cell_length_c                   13.5436(11)
_cell_measurement_reflns_used    9486
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.01
_cell_measurement_theta_min      2.46
_cell_volume                     2472.3(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_detector       'Dectris PILATUS 6M'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72929
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19112
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.812
_diffrn_reflns_theta_max         25.812
_diffrn_reflns_theta_min         2.461
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.0922
_exptl_absorpt_correction_T_min  0.0385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1636 before and 0.1036 after correction.
The Ratio of minimum to maximum transmission is 0.4176.
The \l/2 correction factor is 0.00400.
;
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1387P)^2^+2.1593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.1906
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3963
_reflns_number_total             4111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-1195463.cif
_cod_data_source_block           js173
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1565161
_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
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C11(H11), C13(H13), C14(H14), C20(H20)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'