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_7710200
_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         'C93 H63 Cl3 N42 Ni3, 9.294(O), 1.301(C O)'
_chemical_formula_sum            'C94.3 H63 Cl3 N42 Ni3 O10.6'
_chemical_formula_weight         2236.48
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                120
_cell_formula_units_Z            6
_cell_length_a                   19.7747(6)
_cell_length_b                   19.7747(6)
_cell_length_c                   48.334(2)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      65.01
_cell_measurement_theta_min      2.74
_cell_volume                     16368.3(10)
_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_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0990
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            41376
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        65.267
_diffrn_reflns_theta_max         65.267
_diffrn_reflns_theta_min         2.737
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dull brownish black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             6855
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00056(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1852P)^2^+0.9493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4601
_reflns_number_total             6123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00221c2.cif
_cod_data_source_block           ni3
_cod_original_cell_volume        16368.2(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C94.30 H63 Cl3 N42 Ni3 O10.60'
_cod_database_code               7710200
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(O6)=1-FVAR(1)
 Sof(O1)=0.33333*(1-FVAR(2))
 Sof(O4)=Sof(C32)=FVAR(1)
 Sof(O5)=1-FVAR(2)
 Sof(O3)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C1(H1), C5(H5), C26(H26), C3(H3), C20(H20), C4(H4), C21(H21),
 C2(H2), C12(H12), C22(H22), C29(H29), C13(H13), C23(H23), C16(H16), C28(H28),
 C24(H24), C19(H19), C18(H18), C17(H17)
;
_shelx_res_checksum              72734
_shelx_hkl_checksum              34774
_olex2_submission_special_instructions 'No special instructions were received'