The crystal structure of bis((E)-2-((tert-butylimino)methyl)-4-chlorophenolato-κ2 N,O)zinc(II), C22H26Cl2N2O2Zn
Yang, Qian-Zhi; Yang, Yu-Xin; Kuang, Jin-Hao; Li, Zhong-Yan; Lin Yuan,; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 425–427; doi:10.1515/ncrs-2022-0049

data_8105714
_publ_section_title
;
 The crystal structure of
 bis((E)-2-((tert-butylimino)methyl)-4-chlorophenolato-\k2 N,O)zinc(II),
 C22H26Cl2N2O2Zn
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              425
_journal_page_last               427
_journal_paper_doi               10.1515/ncrs-2022-0049
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C22 H26 Cl2 N2 O2 Zn'
_chemical_formula_sum            'C22 H26 Cl2 N2 O2 Zn'
_chemical_formula_weight         486.72
_chemical_name_systematic
;
The crystal structure of (E)-2-((tert-butylimino)methyl)-4-chlorophenol Zinc
Complex 
;
_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                 99.705(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.488(7)
_cell_length_b                   10.139(7)
_cell_length_c                   22.760(15)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.20
_cell_volume                     2386(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21975
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.815
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1049 before and 0.0376 after correction.
The Ratio of minimum to maximum transmission is 0.7543.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0444
_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/[\s^2^(Fo^2^)+(0.0376P)^2^+2.9448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3749
_reflns_number_total             4208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0049_suppl.cif
_cod_data_source_block           2
_cod_database_code               8105714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C7(H7), C3(H3), C17(H17), C15(H15), C6(H6), C4(H4), C14(H14)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C9(H9A,H9B,
 H9C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              38759
_shelx_hkl_checksum              83653