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_4322759
_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        Dichloromethane/Acetonitrile
_chemical_formula_sum            'C199 H213.5 B4 Cl4 N36.5 Ni O8 Zn4'
_chemical_formula_weight         3749.79
_chemical_name_systematic
;
 Tetrakis[hydrotris(3-cumenyl-5-methyl-pyrazol-1-yl)borato-zink(II)-
 2,9,16,23-tetraoxo-3,10,17,24-tetrahydroxo-phtaloocyaninatonickel(II)
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                108.238(9)
_cell_angle_beta                 116.276(8)
_cell_angle_gamma                95.711(8)
_cell_formula_units_Z            1
_cell_length_a                   18.099(3)
_cell_length_b                   18.415(4)
_cell_length_c                   18.466(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    161(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      0
_cell_volume                     5032.5(17)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens XSCANS'
_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      161(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  0.0884
_diffrn_reflns_av_sigmaI/netI    0.1195
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35685
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1963
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.394
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.205
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1309
_refine_ls_number_reflns         13881
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.202
_refine_ls_R_factor_all          0.1825
_refine_ls_R_factor_obs          0.1110
_refine_ls_shift/esd_max         0.740
_refine_ls_shift/esd_mean        0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2210P)^2^+1.2430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3601
_refine_ls_wR_factor_obs         0.2936
_reflns_number_observed          7612
_reflns_number_total             13924
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980036g_5.cif
_cod_data_source_block           ruf004
_cod_original_cell_volume        5032.3(16)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4322759