Interrelationships between the tetrahedral and planar polymorphs of bis(3-ethylamino-1-phenyl-but-2-en-1-ono)nickel(ii) and structural comparisons with related CoII, NiII, CuII, and ZnII complexes
Powers, Xian B.; Ghiassi, Kamran B.; Greenfield, Joshua T.; Olmstead, Marilyn M.; Balch, Alan L.; CrystEngComm  (2017) –; doi:10.1039/C7CE00638A

data_7228168
_publ_section_title
;
 Interrelationships between the tetrahedral and planar polymorphs of
 bis(3-ethylamino-1-phenyl-but-2-en-1-ono)nickel(ii) and structural
 comparisons with related CoII, NiII, CuII, and ZnII complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00638A
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H32 Co N2 O2'
_chemical_formula_sum            'C34 H32 Co N2 O2'
_chemical_formula_weight         559.54
_chemical_name_common            Co(B-Bn)2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-17 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1696(16)
_cell_length_b                   16.2061(17)
_cell_length_c                   5.6087(6)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.43
_cell_measurement_theta_min      2.51
_cell_volume                     1378.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'Apex2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            23476
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.717
_diffrn_reflns_theta_min         1.839
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.011(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0358P)^2^+0.1111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4338
_reflns_number_total             4637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00638a1.cif
_cod_data_source_block           xbp36
_cod_database_code               7228168
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              82978