Photo-activation of d(0) niobium imido azides: en route to nitrido complexes.
Camp, Clément; Grant, Lauren N.; Bergman, Robert G.; Arnold, John; Chemical communications (Cambridge, England) 52 (2016) 5538–5541; doi:10.1039/c6cc02081j

data_7124620
_publ_section_title
;
 Photo-activation of d(0) niobium imido azides: en route to nitrido
 complexes.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5538
_journal_page_last               5541
_journal_paper_doi               10.1039/c6cc02081j
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C39 H54 N3 Nb'
_chemical_formula_weight         657.76
_chemical_name_common            (BDI)Nb(NtBu)Ph
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           shelxl-2014
_audit_update_record
;
2016-03-08 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                107.0190(10)
_cell_angle_beta                 113.6050(10)
_cell_angle_gamma                91.5850(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6363(4)
_cell_length_b                   10.3540(4)
_cell_length_c                   10.4978(4)
_cell_measurement_temperature    100(2)
_cell_volume                     905.11(6)
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'shelxl-2014 (sheldrick, 2014)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12336
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         2.086
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       plates
_exptl_crystal_F_000             350
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 flack x determined using 2318 quotients [(i+)-(i-)]/[(i+)+(i-)]
 (parsons, flack and wagner, acta cryst. b69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.089(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5814
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(fo^2^)+(0.0318p)^2^+0.3065p] where p=(fo^2^+2fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.765
_reflns_Friedel_fraction_max     0.746
_reflns_number_gt                5687
_reflns_number_total             5814
_reflns_threshold_expression     'i > 2\s(i)'
_cod_data_source_file            c6cc02081j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_site_adp_type' value 'uani' was changed to 'Uani' in
accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (43 times).

data item '_atom_site_adp_type' value 'uiso' was changed to 'Uiso' in
accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (54 times).

data item '_atom_site_refinement_flags_adp' value 'u' was changed to
'U' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (54 times).

data item '_atom_site_refinement_flags_posn' value 'r' was changed to
'R' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (54 times).

data item '_refine_ls_structure_factor_coef' value 'fsqd' was changed
to 'Fsqd' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/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_Hall     'p 1'
_cod_original_sg_symbol_H-M      'p 1'
_cod_database_code               7124620
_shelx_estimated_absorpt_t_min   0.869
_shelx_estimated_absorpt_t_max   0.965
_shelxl_version_number           2014-1
_shelx_res_checksum              30857
_shelx_hkl_checksum              6319