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_1559886
_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         'C44 H44 N4 O8 Ni2, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H50 N6 Ni2 O8'
_chemical_formula_weight         956.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 91.4245(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8061(5)
_cell_length_b                   10.1122(4)
_cell_length_c                   15.8955(6)
_cell_measurement_reflns_used    9753
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.39
_cell_volume                     2218.49(15)
_computing_cell_refinement       'Bruker SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker APEX3 v2019.2-37 (Bruker, 2019)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture Photon-II'
_diffrn_measurement_method       '\w-\f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75810
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         2.497
_diffrn_source                   'Incoatec Mo-microfocus 3.0'
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.821
_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            colorless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       rod
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0154P)^2^+2.1278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4695
_reflns_number_total             5511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ed0c01117_si_011.cif
_cod_data_source_block           Ni(salophen)(HOAc)-dimer
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1559886
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              64003
_shelx_hkl_checksum              22108