Coordination Compounds of Niobium(IV) Oxide Dihalides Including the Synthesis and the Crystallographic Characterization of NHC Complexes.
Bortoluzzi, Marco; Ferretti, Eleonora; Marchetti, Fabio; Pampaloni, Guido; Pinzino, Calogero; Zacchini, Stefano; Inorganic chemistry 55 (2016) 4173–4182; doi:10.1021/acs.inorgchem.5b02888

data_4347208
_publ_section_title
;
 Coordination Compounds of Niobium(IV) Oxide Dihalides Including the
 Synthesis and the Crystallographic Characterization of NHC Complexes.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4173
_journal_page_last               4182
_journal_paper_doi               10.1021/acs.inorgchem.5b02888
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C45 H55 Cl2 N4 Nb O'
_chemical_formula_weight         831.74
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_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                 100.206(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.131(6)
_cell_length_b                   12.795(2)
_cell_length_c                   24.138(5)
_cell_measurement_reflns_used    4664
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.082
_cell_measurement_theta_min      2.351
_cell_volume                     9159(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43118
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.9366
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.0927 (selected reflections only, before parameter refinement)
 R(int) =  0.0619 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            brown-green
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.981
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         8988
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1393P)^2^+35.4388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2062
_refine_ls_wR_factor_ref         0.2383
_reflns_number_gt                6202
_reflns_number_total             8988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02888_si_002.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4347208