Bite-Angle-Regulated Coordination Geometries: Tetrahedral and Trigonal Bipyramidal in Ni(II) with Biphenyl-Appended (2-Pyridyl)alkylamine <i>N</i>,<i>N</i>'-Bidentate Ligands.
Sasi, Divya; Ramkumar, Venkatachalam; Murthy, Narasimha N.; ACS omega 2 (2017) 2474–2481; doi:10.1021/acsomega.7b00119

data_4516846
_publ_section_title
;
 Bite-Angle-Regulated Coordination Geometries: Tetrahedral and Trigonal
 Bipyramidal in Ni(II) with Biphenyl-Appended (2-Pyridyl)alkylamine
 <i>N</i>,<i>N</i>'-Bidentate Ligands.
;
_journal_issue                   6
_journal_name_full               'ACS omega'
_journal_page_first              2474
_journal_page_last               2481
_journal_paper_doi               10.1021/acsomega.7b00119
_journal_volume                  2
_journal_year                    2017
_chemical_formula_moiety         'C41 H38 Br Cl3 N4 Ni O4'
_chemical_formula_sum            'C41 H38 Br Cl3 N4 Ni O4'
_chemical_formula_weight         895.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.680(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9042(9)
_cell_length_b                   14.4103(9)
_cell_length_c                   19.0672(9)
_cell_measurement_reflns_used    7907
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.40
_cell_volume                     4010.3(4)
_computing_cell_refinement       'APEX II, Bruker, 2004'
_computing_data_collection       'APEX II, Bruker, 2004'
_computing_data_reduction        'SAINT, Bruker, 2004'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2013)'
_computing_publication_material  'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.623
_diffrn_measurement_device_type  'Bruker ApexII ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29514
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.73
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  0.7818
_exptl_absorpt_correction_T_min  0.5833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Bruker,2004)
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9210
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+4.8589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                6182
_reflns_number_total             9210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao7b00119_si_002.cif
_cod_data_source_block           C41H38BrCl3N4NiO4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4516846