Reduction of carbon monoxide by a tetrakis(aryloxide)diniobium complex having four bridging hydrides.
Kurogi, Takashi; Ishida, Yutaka; Hatanaka, Tsubasa; Kawaguchi, Hiroyuki; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7510–7513; doi:10.1039/c2dt32798h

data_7021337
_publ_section_title
;
 Reduction of carbon monoxide by a tetrakis(aryloxide)diniobium complex
 having four bridging hydrides.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7510
_journal_page_last               7513
_journal_paper_doi               10.1039/c2dt32798h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C109 H142 Nb2 O5, 3.5(C7 H8)'
_chemical_formula_sum            'C133.5 H170 Nb2 O5'
_chemical_formula_weight         2040.52
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.185(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.333(3)
_cell_length_b                   25.833(5)
_cell_length_c                   21.541(4)
_cell_measurement_reflns_used    12187
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4507
_cell_measurement_theta_min      3.1074
_cell_volume                     11315(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Saturn CCD (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69689
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.9873
_exptl_absorpt_correction_T_min  0.9723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4372
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         12895
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+25.9946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                10013
_reflns_number_total             12895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32798h.txt
_cod_data_source_block           '[{(ArO)2Nb}2(CH2)(O)](toluene)3.5'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        11314(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C133.50 H170 Nb2 O5'
_cod_database_code               7021337