Phthalocyanine as a Chemically Inert, Redox-Active Ligand: Structural and Electronic Properties of a Nb(IV)-Oxo Complex Incorporating a Highly Reduced Phthalocyanine(4-) Anion
Edwin W. Y. Wong; Charles J. Walsby; Tim Storr; Daniel B. Leznoff; Inorganic Chemistry 49 (2010) 3343–3350; doi:10.1021/ic902409n

data_4315295
_publ_contact_author_address
; 
Leznoff, Daniel B.
Department of Chemistry
Simon Fraser University
Burnaby, British Columbia
Canada         V5A 1S6
;
_publ_contact_author_email       dleznoff@sfu.ca
_publ_contact_author_fax         +1-778-782-3765
_publ_contact_author_name        'Daniel B. Leznoff'
_publ_contact_author_phone       +1-778-782-4887
_publ_section_title
;
 Phthalocyanine as a Chemically Inert, Redox-Active Ligand: Structural and
 Electronic Properties of a Nb(IV)-Oxo Complex Incorporating a Highly
 Reduced Phthalocyanine(4-) Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3343
_journal_page_last               3350
_journal_paper_doi               10.1021/ic902409n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C52 H66.00 K2 N8 Nb1 O11'
_chemical_formula_sum            'C52 H66 K2 N8 Nb O11'
_chemical_formula_weight         1150.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 106.131(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.832(2)
_cell_length_b                   20.841(3)
_cell_length_c                   18.778(3)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.26
_cell_volume                     5576.0(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994)
 CRYSTALS (Watkin, 1988) 
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62442
_diffrn_reflns_theta_full        27.062
_diffrn_reflns_theta_max         28.486
_diffrn_reflns_theta_min         1.731
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6167
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark purple/green'
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.80
_refine_diff_density_min         -1.41
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1739
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.000576
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0714
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0524
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7226
_reflns_number_total             13145
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0543
_oxford_refine_ls_scale          0.07003(8)
_oxford_reflns_number_all        13145
_oxford_reflns_threshold_expression_ref I>2.5\s(I)
_cod_data_source_file            ic902409n_si_002_2.cif
_cod_data_source_block           DME
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5576.3(13)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C52 H66.00 K2 N8 Nb1 O11'
_cod_database_code               4315295