Coordination-driven assembly of a supramolecular square and oxidation to a tetra-ligand radical species
Herasymchuk, Khrystyna; Miller, Jessica J.; MacNeil, Gregory; Sergeenko, Ania; McKearney, Declan; Goeb, Sebastien; Salle, Marc; Leznoff, Daniel B.; Storr, Tim; Chemical Communications  (2019) –; doi:10.1039/C9CC02320H

data_7123353
_publ_section_title
;
 Coordination-driven assembly of a supramolecular square and oxidation to
 a tetra-ligand radical species
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02320H
_journal_year                    2019
_chemical_formula_sum            'C38 H42 N4 Ni O2'
_chemical_formula_weight         645.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2019-03-14 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                102.6010(10)
_cell_angle_beta                 107.7680(10)
_cell_angle_gamma                112.9790(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0566(3)
_cell_length_b                   12.9924(3)
_cell_length_c                   13.9528(3)
_cell_measurement_reflns_used    9238
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      66.61
_cell_measurement_theta_min      3.60
_cell_volume                     1622.03(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1725
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30617
_diffrn_reflns_theta_full        66.707
_diffrn_reflns_theta_max         66.707
_diffrn_reflns_theta_min         3.604
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick , 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.400
_refine_ls_extinction_coef       0.0114(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         5556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+2.4326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.1983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5107
_reflns_number_total             5556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02320h2.cif
_cod_data_source_block           KH_3_144_py
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1622.02(7)
_cod_database_code               7123353
_shelx_estimated_absorpt_t_min   0.745
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              56668