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_4322756
_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_compound_source        methanol/dichloromethane
_chemical_formula_sum            'C49.5 H56 B Cl3 N7 O5 Zn'
_chemical_formula_weight         1011.54
_chemical_name_common            Tp^Cum,Me^Zn(HphCat)
_chemical_name_systematic
;
 Hydrotris(3-cumenyl-5-methyl-pyrazol-1-yl)borato-zinc-
5-hydroxy-6-oxo-phtalimide
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.043(2)
_cell_length_b                   16.378(2)
_cell_length_c                   29.347(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    166(2)
_cell_measurement_theta_max      32
_cell_measurement_theta_min      0
_cell_volume                     10114(2)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      166(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            64407
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       rod
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.109
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         9803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_restrained_S_obs      1.109
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_obs          0.0573
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+15.9642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1585
_refine_ls_wR_factor_obs         0.1377
_reflns_number_observed          7864
_reflns_number_total             9932
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980036g_2.cif
_cod_data_source_block           ruf10
_cod_original_cell_volume        10114.1(21)
_cod_original_formula_sum        'C49.50 H56 B Cl3 N7 O5 Zn'
_cod_database_code               4322756