Metal effects on ligand non-innocence in Group 5 complexes of the redox-active [ONO] pincer ligand.
Hananouchi, Steven; Krull, Brandon T.; Ziller, Joseph W.; Furche, Filipp; Heyduk, Alan F.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 17991–18000; doi:10.1039/c4dt02259a

data_7032939
_publ_section_title
;
 Metal effects on ligand non-innocence in Group 5 complexes of the
 redox-active [ONO] pincer ligand.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17991
_journal_page_last               18000
_journal_paper_doi               10.1039/c4dt02259a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C37 H62 Cl2 N Nb O3'
_chemical_formula_weight         732.68
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_a                   14.5710(10)
_cell_length_b                   15.9423(11)
_cell_length_c                   17.0831(12)
_cell_measurement_reflns_used    9357
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.24
_cell_volume                     3968.3(5)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'Bruker SHELXTL 2008/4'
_diffrn_ambient_temperature      143(2)
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_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0172
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_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
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_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45745
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.506
_diffrn_reflns_theta_min         1.747
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  0.9450
_exptl_absorpt_correction_T_min  0.8456
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.174
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_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.38(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         9374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+1.1694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                9111
_reflns_number_total             9374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02259a2.cif
_cod_data_source_block           afh295
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7032938--7032941.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               7032939
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.923
_shelxl_version_number           2014-2
_shelx_res_checksum              3616
_shelx_hkl_checksum              55116