Novel Seven Coordination Geometry of Sn(IV): Crystal Structures of Phthalocyaninato Bis(undecylcarboxylato)Sn(IV), Its Si(IV) Analogue, and Phthalocyaninato Bis(chloro)silicon(IV). The Electrochemistry of the Si(IV) Analogue and Related Compounds
Jack Silver; Christopher S. Frampton; George R. Fern; Dominic A. Davies; John R. Miller; Jose L. Sosa-Sanchez; Inorganic Chemistry 40 (2001) 5434–5439; doi:10.1021/ic001120a

data_4320340
_publ_contact_author
;
Dr Christopher S. Frampton
Department of Chemistry
Roche Discovery Welwyn
Welwyn Garden City
Hertfordshire
AL7 3AY
U.K.
;
_publ_contact_author_email       christopher.frampton@roche.com
_publ_contact_author_fax         44(1707)366907
_publ_contact_author_phone       44(1707)366272
_publ_section_title
;
 Novel Seven Coordination Geometry of Sn(IV): Crystal Structures of
 Phthalocyaninato Bis(undecylcarboxylato)Sn(IV), Its Si(IV) Analogue, and
 Phthalocyaninato Bis(chloro)silicon(IV). The Electrochemistry of the
 Si(IV) Analogue and Related Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5434
_journal_page_last               5439
_journal_paper_doi               10.1021/ic001120a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C56 H62 N8 O4 Si'
_chemical_formula_weight         939.23
_chemical_name_systematic
; 
Phthalocyaninato bis(undecylcarboxylato)Silicon(IV) 
;
_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                105.797(10)
_cell_angle_beta                 100.621(11)
_cell_angle_gamma                93.939(12)
_cell_formula_units_Z            2
_cell_length_a                   8.9976(14)
_cell_length_b                   15.522(2)
_cell_length_c                   19.031(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      1.50
_cell_volume                     2493.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(1)
_diffrn_measurement_device_type  'Enraf-Nonius CAD4R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9059
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         8769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1508
_reflns_number_gt                5182
_reflns_number_total             8769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001120a_1.cif
_cod_data_source_block           newg6
_cod_original_cell_volume        2493.9(6)
_cod_database_code               4320340