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_4315294
_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_absolute_configuration ad
_chemical_formula_moiety         'C60.00 H74 K2 N8 Nb1.00 O15.00'
_chemical_formula_sum            'C60 H74 K2 N8 Nb O15'
_chemical_formula_weight         1318.39
_space_group_IT_number           1
_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
_cell_angle_alpha                89.856(2)
_cell_angle_beta                 75.837(2)
_cell_angle_gamma                69.397(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1153(18)
_cell_length_b                   11.6215(19)
_cell_length_c                   13.624(2)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.21
_cell_volume                     1590.5(4)
_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      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18520
_diffrn_reflns_theta_full        25.901
_diffrn_reflns_theta_max         28.463
_diffrn_reflns_theta_min         1.880
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark purple/green'
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       chunk
_exptl_crystal_F_000             689
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details 'Flack (1983), 6555 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0318
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         13595
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.000898
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.238 0.234 0.574E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0683
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0567
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_gt                13630
_reflns_number_total             13862
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.08
_oxford_diffrn_Wilson_scale      75.02
_oxford_refine_ls_r_factor_ref   0.0500
_oxford_refine_ls_scale          0.1405(2)
_oxford_reflns_number_all        13862
_oxford_reflns_threshold_expression_ref I>2.5\s(I)
_cod_data_source_file            ic902409n_si_002_1.cif
_cod_data_source_block           18-crown-6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      'P 1 '
_cod_original_formula_sum        'C60.00 H74 K2 N8 Nb1.00 O15.00'
_cod_database_code               4315294