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_1565159
_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         'C22 H30 Cl2 Hg N4 O2, 0.5[C2H6O]'
_chemical_formula_sum            'C23 H33 Cl2 Hg N4 O2.5'
_chemical_formula_weight         677.02
_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                 99.661(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1617(19)
_cell_length_b                   13.094(2)
_cell_length_c                   18.698(4)
_cell_measurement_reflns_used    529
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.21
_cell_measurement_theta_min      2.70
_cell_volume                     2694.0(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker Apex3 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1006
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37205
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.418
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.940
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1071 before and 0.0723 after correction.
The Ratio of minimum to maximum transmission is 0.6040.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0227P)^2^+7.4982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3161
_reflns_number_total             4760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-1195461.cif
_cod_data_source_block           js250
_cod_original_cell_volume        2693.8(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C23 H33 Cl2 Hg N4 O2.50'
_cod_database_code               1565159
_shelx_estimated_absorpt_t_max   0.648
_shelx_estimated_absorpt_t_min   0.588
_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:
 C17(H17A,H17B), C6(H6A,H6B), C15(H15A,H15B), C16(H16A,H16B), C7(H7A,H7B),
 C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C20(H20), C3(H3), C11(H11), C10(H10)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62269
_shelx_hkl_checksum              89218
_shelx_fab_checksum              61824
_olex2_submission_special_instructions 'No special instructions were received'