Toward the Design of Phosphorescent Emitters of Cyclometalated Earth-Abundant Nickel(II) and Their Supramolecular Study.
Wong, Yip-Sang; Tang, Man-Chung; Ng, Maggie; Yam, Vivian Wing-Wah; Journal of the American Chemical Society 142 (2020) 7638–7646; doi:10.1021/jacs.0c02172

data_4134688
_publ_section_title
;
 Toward the Design of Phosphorescent Emitters of Cyclometalated
 Earth-Abundant Nickel(II) and Their Supramolecular Study.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7638
_journal_page_last               7646
_journal_paper_doi               10.1021/jacs.0c02172
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C24 H16 N2 Ni O'
_chemical_formula_sum            'C24 H16 N2 Ni O'
_chemical_formula_weight         407.10
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-13
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.472(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4673(8)
_cell_length_b                   11.3216(9)
_cell_length_c                   32.085(3)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100.04
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.21
_cell_volume                     3409.8(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.04
_diffrn_detector                 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            31178
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.598
_diffrn_reflns_theta_min         2.561
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0726 before and 0.0536 after correction. The Ratio of minimum to maximum transmission is 0.7709. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0457P)^2^+5.9798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6849
_reflns_number_total             7794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02172_si_003.cif
_cod_data_source_block           z1
_cod_depositor_comments
'Adding full bibliography for 4134688--4134689.cif.'
_cod_database_code               4134688
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C37(HG,HH), C15(H15A,H15B), C36(HK,HL)
2.b Aromatic/amide H refined with riding coordinates:
 C41(H), C25(HA), C40(HB), C22(H22), C1(H1), C7(H7), C4(H4), C23(H23),
 C17(H17), C16(H16), C31(HC), C26(HD), C8(H8), C32(HE), C44(HF), C28(HI),
 C3(H3), C27(HJ), C2(H2), C20(H20), C21(H21), C45(HM), C46(HN), C47(HO)
;
_shelx_res_checksum              44438
_shelx_hkl_checksum              22116
_olex2_submission_special_instructions 'No special instructions were received'