Multiweek Experiments for an Inorganic Chemistry Laboratory Course: Synthesis of Nickel Complexes Supported by a Tetradentate Ligand with a N2O2 Donor Set
Collett, Joel D.; Krause, Jeanette A.; Guan, Hairong; Journal of Chemical Education  (2020) –; doi:10.1021/acs.jchemed.0c01117

data_1559887
_publ_section_title
;
 Multiweek Experiments for an Inorganic Chemistry Laboratory Course:
 Synthesis of Nickel Complexes Supported by a Tetradentate Ligand with a
 N2O2 Donor Set
;
_journal_name_full               'Journal of Chemical Education'
_journal_paper_doi               10.1021/acs.jchemed.0c01117
_journal_year                    2020
_chemical_formula_moiety         'C20 H14 N2 Ni O2'
_chemical_formula_sum            'C20 H14 N2 Ni O2'
_chemical_formula_weight         373.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.36239(9)
_cell_length_b                   16.6313(3)
_cell_length_c                   17.2165(3)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.55
_cell_measurement_theta_min      3.69
_cell_volume                     1535.43(5)
_computing_cell_refinement       'Bruker SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker APEX3 v2018.7.2 (Bruker, 2018)'
_computing_data_reduction        'Bruker SAINT v8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement
'SHELXL-2017/1 (Sheldrick, 2018, G.M. Sheldrick (2015) Acta Cryst., C71, 3-8)'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Photon-II'
_diffrn_measurement_method       '\w-\f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18441
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.559
_diffrn_reflns_theta_min         3.695
_diffrn_source                   'Incoatec Cu-microfocus 3.0'
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2016/2 (L.Krause, et al. J. Appl. Cryst. (2015), 48, 3-10)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).

Flack parameter is negative, meaningless.
;
_refine_ls_abs_structure_Flack   -0.024(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0397P)^2^+0.1892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.702
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3064
_reflns_number_total             3134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ed0c01117_si_010.cif
_cod_data_source_block           20028c
_cod_original_cell_volume        1535.43(4)
_cod_database_code               1559887
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              76833
_shelx_hkl_checksum              82011