Silicon and Zinc Coordination to Peripheral Catechol Sites of (2,3,9,10,16,17,23,24-Octahydroxyphthalocyaninato)nickel(II). Phthalocyanine Coordination Chemistry at the Edge
Michael Ruf; Andrew M. Lawrence; Bruce C. Noll; Cortlandt G. Pierpont; Inorganic Chemistry 37 (1998) 1992–1999; doi:10.1021/ic980036g

data_4322757
_publ_section_title
;
 Silicon and Zinc Coordination to Peripheral Catechol Sites of
 (2,3,9,10,16,17,23,24-Octahydroxyphthalocyaninato)nickel(II).
 Phthalocyanine Coordination Chemistry at the Edge
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1992
_journal_page_last               1999
_journal_paper_doi               10.1021/ic980036g
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C53.75 H72 B N8 O6.75 Zn'
_chemical_formula_weight         1014.37
_chemical_name_common            Tp^Cum,Me^Zn(PhCat)
_chemical_name_systematic
;
 Hydrotris(3-cumenyl-5-methyl-pyrazol-1-yl)borato-
 zinc-5,6-dioxo-phtalimide]tetramethylammonium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   '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                 106.781(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.623(5)
_cell_length_b                   14.197(3)
_cell_length_c                   24.602(5)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    171(2)
_cell_measurement_theta_max      31.31
_cell_measurement_theta_min      0
_cell_volume                     5559(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      171(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            49355
_diffrn_reflns_theta_full        31.31
_diffrn_reflns_theta_max         31.31
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_correction_T_min  0.6919
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange/red
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2158
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         16869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.219
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+4.8678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                12659
_reflns_number_total             16869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980036g_3.cif
_cod_data_source_block           ruf019
_cod_database_code               4322757