Template synthesis and X-ray crystal structures of 15-membered unsymmetric monobenzotetraazaannulene nickel(II) complexes
Eunhee Kim; Hyosun Lee; Inorganica Chimica Acta 399 (2013) 62–66; doi:

data_1516850
_publ_section_title
;
 Template synthesis and X-ray crystal structures of 15-membered
 unsymmetric monobenzotetraazaannulene nickel(II) complexes
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              62
_journal_page_last               66
_journal_volume                  399
_journal_year                    2013
_chemical_formula_sum            'C31 H32 N4 Ni'
_chemical_formula_weight         519.31
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                104.5020(10)
_cell_angle_beta                 99.8040(10)
_cell_angle_gamma                111.8220(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5642(7)
_cell_length_b                   12.4445(9)
_cell_length_c                   12.6253(10)
_cell_measurement_reflns_used    4207
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.52
_cell_volume                     1291.28(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  '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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7531
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+1.8264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                4349
_reflns_number_total             5183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-399-62-66-1.cif
_cod_data_source_block           a1
_cod_depositor_comments
;

2017-03-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1291.27(17)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C62 H64 N8 Ni2'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1038.63
_cod_database_code               1516850