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_1565164
_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 Cd Cl2 N4 O2, 0.5[C2H6O]'
_chemical_formula_sum            'C23 H33 Cd Cl2 N4 O2.5'
_chemical_formula_weight         588.83
_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                 101.2850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1004(3)
_cell_length_b                   12.9995(3)
_cell_length_c                   18.6202(5)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.29
_cell_volume                     2634.94(12)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker Apex3, 2018'
_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 0.991
_diffrn_measured_fraction_theta_max 0.989
_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  0.0945
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5995
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         1.923
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.745684
_exptl_absorpt_correction_T_min  0.349755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 75830 reflections, Rint = 0.1010
 (40507 with I > 3sig(I), Rint = 0.0945)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
TITL js108r1_a        P 1 21/n 1   R = 0.07
CELL   11.1004   12.9995   18.6202     90.00    101.29     90.00
SPGR P21/n
C101 0.517 0.053 0.408 !       3.78 eA-3
C102 0.580 0.914 0.391 !       3.25 eA-3
C103 1.003 0.462 0.097 !       3.21 eA-3
C104 0.534 0.076 0.332 !       2.95 eA-3
Q105 1.002 0.103 0.262 !       1.95 eA-3
Q106 0.126 0.098 0.233 !       1.91 eA-3
Q107 0.377 0.561 0.225 !       1.33 eA-3
Q108 0.438 0.547 0.301 !       1.28 eA-3
Q109 0.607 0.487 0.731 !       1.21 eA-3
Q110 0.107 0.178 0.233 !       1.19 eA-3
Q111 0.468 0.486 0.283 !       1.16 eA-3
Q112 0.986 0.977 0.733 !       1.09 eA-3
Q113 0.951 0.877 0.792 !       1.07 eA-3
Q114 0.059 0.442 0.159 !       1.01 eA-3
Q115 0.535 0.299 0.727 !       0.99 eA-3
Q116 0.674 0.089 0.832 !       0.85 eA-3
Q117 0.594 0.516 0.781 !       0.84 eA-3
Q118 0.984 0.047 0.227 !       0.81 eA-3
Q119 0.485 0.670 0.234 !       0.81 eA-3
Q120 0.479 0.389 0.594 !       0.79 eA-3
Q121 0.358 0.329 0.692 !       0.78 eA-3
Q122 0.405 0.814 0.297 !       0.78 eA-3
Q123 0.999 0.605 0.951 !       0.76 eA-3
Q124 0.656 0.981 0.527 !       0.74 eA-3
Q125 0.172 0.772 0.840 !       0.74 eA-3
Q126 0.031 0.179 0.583 !       0.70 eA-3
Q127 0.469 0.665 0.926 !       0.70 eA-3
Q128 0.421 0.313 0.756 !       0.70 eA-3
Q129 0.687 0.948 0.720 !       0.69 eA-3
Q130 0.080 0.217 0.184 !       0.68 eA-3
C131 0.012 0.385 0.124 !       0.67 eA-3
Q132 0.611 0.841 0.251 !       0.67 eA-3
Q133 0.097 0.830 0.036 !       0.67 eA-3
Q134 0.903 0.170 0.964 !       0.67 eA-3
Q135 0.409 0.924 0.387 !       0.66 eA-3
Q136 0.999 0.970 0.342 !       0.65 eA-3
Q137 0.014 0.757 0.909 !       0.65 eA-3
Q138 0.405 0.626 0.201 !       0.65 eA-3
Q139 0.982 0.094 0.795 !       0.65 eA-3
Q140 0.908 0.601 0.061 !       0.64 eA-3
Q141 0.875 0.169 0.989 !       0.63 eA-3
Q142 0.237 0.902 0.856 !       0.63 eA-3
Q143 0.861 0.222 0.192 !       0.63 eA-3
Q144 0.984 0.952 0.171 !       0.63 eA-3
Q145 0.579 0.878 0.470 !       0.61 eA-3
Q146 0.952 0.325 0.933 !       0.61 eA-3
Q147 0.800 0.804 0.470 !       0.61 eA-3
Q148 0.403 0.468 0.740 !       0.60 eA-3
Q149 0.529 0.388 0.330 !       0.60 eA-3
Q150 0.240 0.126 0.343 !       0.60 eA-3
Q151 0.628 0.117 0.530 !       0.60 eA-3
Q152 0.980 0.320 0.313 !       0.60 eA-3
Q153 0.578 0.907 0.111 !       0.59 eA-3
Q154 0.220 0.269 0.307 !       0.59 eA-3
Q155 0.409 0.044 0.516 !       0.59 eA-3
Q156 0.641 0.414 0.205 !       0.59 eA-3
Q157 0.731 0.049 0.982 !       0.59 eA-3
Q158 0.393 0.420 0.263 !       0.58 eA-3
Q159 0.451 0.839 0.629 !       0.58 eA-3
Q160 0.528 0.640 0.274 !       0.58 eA-3
Q161 0.723 0.409 0.768 !       0.58 eA-3
Q162 0.982 0.413 0.375 !       0.58 eA-3
Q163 0.139 0.317 0.469 !       0.57 eA-3
Q164 0.235 0.760 0.458 !       0.57 eA-3
Q165 0.313 0.186 0.419 !       0.56 eA-3
Q166 0.563 0.949 0.299 !       0.56 eA-3
Q167 0.059 0.349 0.171 !       0.56 eA-3
Q168 0.246 0.581 0.096 !       0.55 eA-3
Q169 0.254 0.075 0.409 !       0.55 eA-3
Q170 0.107 0.462 0.848 !       0.55 eA-3
Q171 0.059 0.594 0.254 !       0.55 eA-3
Q172 0.373 0.186 0.465 !       0.55 eA-3
Q173 0.763 0.419 0.828 !       0.54 eA-3
Q174 0.926 0.234 0.103 !       0.54 eA-3
Q175 0.127 0.892 0.813 !       0.54 eA-3
Q176 0.456 0.897 0.076 !       0.53 eA-3
Q177 0.359 0.963 0.297 !       0.53 eA-3
Q178 0.154 0.959 0.355 !       0.53 eA-3
Q179 0.846 0.041 0.645 !       0.53 eA-3
Q180 1.001 0.962 0.115 !       0.53 eA-3
Q181 0.609 0.036 0.969 !       0.53 eA-3
Q182 0.895 0.978 0.062 !       0.53 eA-3
Q183 0.249 0.149 0.313 !       0.52 eA-3
Q184 0.298 0.909 0.467 !       0.52 eA-3
Q185 0.434 0.240 0.532 !       0.52 eA-3
Q186 0.810 0.466 0.942 !       0.51 eA-3
Q187 0.856 0.106 0.139 !       0.51 eA-3
Q188 0.636 0.249 0.178 !       0.51 eA-3
Q189 0.074 0.841 0.280 !       0.51 eA-3
Q190 0.922 0.727 0.355 !       0.50 eA-3
Q191 0.231 0.386 0.079 !       0.50 eA-3
Q192 0.279 0.266 0.375 !       0.50 eA-3
;
_refine_diff_density_max         1.961
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+2.0730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5443
_reflns_number_total             5995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-1195466.cif
_cod_data_source_block           js108r1_a_sq
_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_original_formula_sum        'C23 H33 Cd Cl2 N4 O2.50'
_cod_database_code               1565164
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.683(4)
 0.317(4)
2. 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
3.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)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C11(H11), C12(H12), C13(H13), C20(H20)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'