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_4322758
_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            'C194 H205 B4 N35 Ni O8 Zn4'
_chemical_formula_weight         3518.36
_chemical_name_common            '[OH)~4~PcNi](OznTp^Cum,Me^)~4~'
_chemical_name_systematic
;
 ?
;
_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-97
_cell_angle_alpha                110.78(3)
_cell_angle_beta                 116.59(3)
_cell_angle_gamma                96.35(2)
_cell_formula_units_Z            1
_cell_length_a                   18.664(5)
_cell_length_b                   17.566(5)
_cell_length_c                   18.708(7)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    161(2)
_cell_measurement_theta_max      31.31
_cell_measurement_theta_min      0
_cell_volume                     4854(4)
_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      161(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  '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  0.0798
_diffrn_reflns_av_sigmaI/netI    0.0936
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            59695
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.9156
_exptl_absorpt_correction_T_min  0.7414
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black/purple
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1846
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.287
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1159
_refine_ls_number_reflns         16754
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1603P)^2^+0.2973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2197
_refine_ls_wR_factor_ref         0.2725
_reflns_number_gt                9451
_reflns_number_total             16754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980036g_4.cif
_cod_data_source_block           ruf18
_cod_original_cell_volume        4854(3)
_cod_database_code               4322758