Self-assembly of Ni(ii) metallacycles (a square and a triangle) supported by tetrazine radical bridges
Wang, Te; Yao, Binling; Guo, Zhilin; Chang, Xiaoyong; Deng, Yi-Fei; Zhang, Yuan-Zhu; Dalton Transactions  (2022) –; doi:10.1039/D2DT00221C

data_7710199
_publ_section_title
;
 Self-assembly of Ni(ii) metallacycles (a square and a triangle) supported
 by tetrazine radical bridges
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00221C
_journal_year                    2022
_chemical_formula_moiety         'C48 H56 N44 Ni4'
_chemical_formula_sum            'C48 H56 N44 Ni4'
_chemical_formula_weight         1484.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-01-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-11 deposited with the CCDC.	2022-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2932(4)
_cell_length_b                   17.2932(4)
_cell_length_c                   41.5378(12)
_cell_measurement_reflns_used    8471
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.00
_cell_measurement_theta_min      4.20
_cell_volume                     12422.1(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            42028
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.152
_diffrn_reflns_theta_max         65.152
_diffrn_reflns_theta_min         4.257
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.997
_exptl_absorpt_correction_T_max  0.1621
_exptl_absorpt_correction_T_min  0.0655
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0954 before and 0.0751 after correction. The Ratio of minimum to maximum transmission is 0.4041. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0576P)^2^+19.9274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2028
_reflns_number_total             2662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00221c2.cif
_cod_data_source_block           ni4
_cod_original_cell_volume        12422.1(7)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               7710199
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.754
_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:
 C3(H3), C10(H10)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              61981
_shelx_hkl_checksum              32102
_olex2_submission_special_instructions 'No special instructions were received'