#------------------------------------------------------------------------------
#$Date: 2019-11-23 16:37:29 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234016 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/46/7124622.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7124622
loop_
_publ_author_name
'Camp, Clément'
'Grant, Lauren N.'
'Bergman, Robert G.'
'Arnold, John'
_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            'C38 H49 N3 Nb'
_chemical_formula_weight         640.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-08 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4801(5)
_cell_length_b                   13.7720(5)
_cell_length_c                   19.2824(8)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.44
_cell_volume                     3314.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (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 0.999
_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  0.1267
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56485
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.400
_diffrn_reflns_theta_min         1.817
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.831
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0406
_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/[σ²(Fo²)+(0.0335P)²+6.8797P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2980
_reflns_number_total             3160
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc02081j2.cif
_cod_data_source_block           shelx
_cod_database_code               7124622
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.859
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.2852(3) 0.5801(3) 0.0000 0.0226(8) Uani 1 2 d S T P
C2 C 0.3056(4) 0.6769(4) 0.0000 0.084(3) Uani 1 2 d S T P
H2 H 0.3780 0.6980 0.0000 0.101 Uiso 1 2 calc R U P
C3 C 0.2246(4) 0.7467(4) 0.0000 0.111(4) Uani 1 2 d S T P
H3 H 0.2432 0.8136 0.0000 0.133 Uiso 1 2 calc R U P
C4 C 0.1204(3) 0.7210(3) 0.0000 0.0412(11) Uani 1 2 d S T P
H4 H 0.0653 0.7686 0.0000 0.049 Uiso 1 2 calc R U P
C5 C 0.0969(3) 0.6245(4) 0.0000 0.0515(14) Uani 1 2 d S T P
H5 H 0.0242 0.6038 0.0000 0.062 Uiso 1 2 calc R U P
C6 C 0.1781(4) 0.5563(3) 0.0000 0.0543(15) Uani 1 2 d S T P
H6 H 0.1591 0.4895 0.0000 0.065 Uiso 1 2 calc R U P
C7 C 0.3610(2) 0.35066(19) 0.14605(13) 0.0238(5) Uani 1 1 d . . .
C8 C 0.4264(3) 0.2711(2) 0.16247(15) 0.0345(7) Uani 1 1 d . . .
C9 C 0.4515(3) 0.2550(2) 0.23196(16) 0.0427(8) Uani 1 1 d . . .
H9 H 0.4945 0.2007 0.2441 0.051 Uiso 1 1 calc R U .
C10 C 0.4153(3) 0.3158(3) 0.28305(16) 0.0442(8) Uani 1 1 d . . .
H10 H 0.4305 0.3019 0.3303 0.053 Uiso 1 1 calc R U .
C11 C 0.3572(2) 0.3968(3) 0.26570(15) 0.0379(7) Uani 1 1 d . . .
H11 H 0.3354 0.4403 0.3013 0.045 Uiso 1 1 calc R U .
C12 C 0.3295(2) 0.4169(2) 0.19713(14) 0.0272(6) Uani 1 1 d . . .
C13 C 0.4660(4) 0.2023(2) 0.10706(17) 0.0593(12) Uani 1 1 d . . .
H13 H 0.4706 0.2398 0.0628 0.071 Uiso 1 1 calc R U .
C14 C 0.3902(5) 0.1171(3) 0.0945(3) 0.105(2) Uani 1 1 d . . .
H14A H 0.4198 0.0751 0.0582 0.158 Uiso 1 1 calc R U .
H14B H 0.3820 0.0798 0.1375 0.158 Uiso 1 1 calc R U .
H14C H 0.3201 0.1417 0.0798 0.158 Uiso 1 1 calc R U .
C15 C 0.5770(5) 0.1625(4) 0.1223(2) 0.0914(19) Uani 1 1 d . . .
H15A H 0.5987 0.1185 0.0849 0.137 Uiso 1 1 calc R U .
H15B H 0.6281 0.2164 0.1254 0.137 Uiso 1 1 calc R U .
H15C H 0.5758 0.1271 0.1663 0.137 Uiso 1 1 calc R U .
C16 C 0.2655(2) 0.5072(2) 0.18069(15) 0.0344(7) Uani 1 1 d . . .
H16 H 0.2670 0.5150 0.1291 0.041 Uiso 1 1 calc R U .
C17 C 0.1495(3) 0.5004(4) 0.2013(3) 0.0832(16) Uani 1 1 d . . .
H17A H 0.1181 0.4413 0.1815 0.125 Uiso 1 1 calc R U .
H17B H 0.1439 0.4981 0.2520 0.125 Uiso 1 1 calc R U .
H17C H 0.1108 0.5573 0.1838 0.125 Uiso 1 1 calc R U .
C18 C 0.3145(3) 0.5973(3) 0.2107(3) 0.0849(17) Uani 1 1 d . . .
H18A H 0.3900 0.6012 0.1970 0.127 Uiso 1 1 calc R U .
H18B H 0.2762 0.6545 0.1932 0.127 Uiso 1 1 calc R U .
H18C H 0.3093 0.5953 0.2614 0.127 Uiso 1 1 calc R U .
C30 C 0.4052(3) 0.5018(3) 0.46400(19) 0.0494(9) Uani 1 1 d . . .
H19 H 0.3394 0.5030 0.4392 0.059 Uiso 1 1 calc R U .
C19 C 0.1850(3) 0.2945(3) 0.0000 0.0266(8) Uani 1 2 d S T P
H20 H 0.1139 0.2700 0.0000 0.032 Uiso 1 2 calc R U P
C20 C 0.2297(2) 0.30999(18) 0.06478(14) 0.0260(6) Uani 1 1 d . . .
C21 C 0.1672(3) 0.2653(3) 0.12397(18) 0.0597(12) Uani 1 1 d . . .
H22A H 0.1035 0.2325 0.1056 0.090 Uiso 1 1 calc R U .
H22B H 0.2124 0.2181 0.1483 0.090 Uiso 1 1 calc R U .
H22C H 0.1452 0.3164 0.1563 0.090 Uiso 1 1 calc R U .
C31 C 0.5000 0.5000 0.4290(3) 0.0544(14) Uani 1 2 d S T P
H25 H 0.5000 0.5000 0.3798 0.065 Uiso 1 2 calc R U P
N1 N 0.5000 0.5000 0.07195(16) 0.0244(7) Uani 1 2 d S T P
N2 N 0.32093(16) 0.35944(14) 0.07590(11) 0.0195(4) Uani 1 1 d . . .
Nb1 Nb 0.39763(2) 0.46044(2) 0.0000 0.01496(12) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 C1 C6 114.6(4) . .
C2 C1 Nb1 128.8(3) . .
C6 C1 Nb1 116.6(3) . .
C1 C2 C3 122.8(4) . .
C1 C2 H2 118.6 . .
C3 C2 H2 118.6 . .
C4 C3 C2 121.2(5) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C3 C4 C5 117.7(4) . .
C3 C4 H4 121.1 . .
C5 C4 H4 121.1 . .
C4 C5 C6 120.3(4) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
C1 C6 C5 123.4(4) . .
C1 C6 H6 118.3 . .
C5 C6 H6 118.3 . .
C8 C7 C12 120.9(3) . .
C8 C7 N2 118.5(2) . .
C12 C7 N2 120.4(2) . .
C9 C8 C7 118.1(3) . .
C9 C8 C13 120.5(3) . .
C7 C8 C13 121.4(3) . .
C10 C9 C8 121.4(3) . .
C10 C9 H9 119.3 . .
C8 C9 H9 119.3 . .
C9 C10 C11 119.7(3) . .
C9 C10 H10 120.1 . .
C11 C10 H10 120.1 . .
C10 C11 C12 121.6(3) . .
C10 C11 H11 119.2 . .
C12 C11 H11 119.2 . .
C11 C12 C7 118.0(3) . .
C11 C12 C16 119.5(3) . .
C7 C12 C16 122.5(2) . .
C8 C13 C14 113.1(4) . .
C8 C13 C15 112.8(3) . .
C14 C13 C15 108.6(3) . .
C8 C13 H13 107.3 . .
C14 C13 H13 107.3 . .
C15 C13 H13 107.3 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C18 C16 C17 110.0(3) . .
C18 C16 C12 112.6(3) . .
C17 C16 C12 113.7(3) . .
C18 C16 H16 106.7 . .
C17 C16 H16 106.7 . .
C12 C16 H16 106.7 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C31 C30 C30 119.7(2) . 6_556
C31 C30 H19 120.2 . .
C30 C30 H19 120.2 6_556 .
C20 C19 C20 128.9(3) . 6
C20 C19 H20 115.5 . .
C20 C19 H20 115.5 6 .
N2 C20 C19 124.3(2) . .
N2 C20 C21 121.5(3) . .
C19 C20 C21 114.2(3) . .
C20 C21 H22A 109.5 . .
C20 C21 H22B 109.5 . .
H22A C21 H22B 109.5 . .
C20 C21 H22C 109.5 . .
H22A C21 H22C 109.5 . .
H22B C21 H22C 109.5 . .
C30 C31 C30 120.6(5) . 2_665
C30 C31 H25 119.7 . .
C30 C31 H25 119.7 2_665 .
Nb1 N1 Nb1 90.07(13) 5_665 .
C20 N2 C7 113.5(2) . .
C20 N2 Nb1 125.03(17) . .
C7 N2 Nb1 121.08(15) . .
N1 Nb1 N1 89.93(13) 5_665 .
N1 Nb1 C1 102.15(7) 5_665 .
N1 Nb1 C1 102.15(7) . .
N1 Nb1 N2 156.12(5) 5_665 .
N1 Nb1 N2 89.35(8) . .
C1 Nb1 N2 101.33(9) . .
N1 Nb1 N2 89.35(8) 5_665 6
N1 Nb1 N2 156.12(5) . 6
C1 Nb1 N2 101.33(9) . 6
N2 Nb1 N2 81.83(10) . 6
N1 Nb1 Nb1 44.97(6) 5_665 5_665
N1 Nb1 Nb1 44.97(6) . 5_665
C1 Nb1 Nb1 107.31(10) . 5_665
N2 Nb1 Nb1 129.66(5) . 5_665
N2 Nb1 Nb1 129.66(5) 6 5_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.356(6) .
C1 C6 1.376(6) .
C1 Nb1 2.165(4) .
C2 C3 1.395(7) .
C2 H2 0.9500 .
C3 C4 1.347(7) .
C3 H3 0.9500 .
C4 C5 1.362(7) .
C4 H4 0.9500 .
C5 C6 1.381(6) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.403(4) .
C7 C12 1.399(4) .
C7 N2 1.447(3) .
C8 C9 1.394(4) .
C8 C13 1.511(4) .
C9 C10 1.369(5) .
C9 H9 0.9500 .
C10 C11 1.373(5) .
C10 H10 0.9500 .
C11 C12 1.394(4) .
C11 H11 0.9500 .
C12 C16 1.512(4) .
C13 C14 1.526(7) .
C13 C15 1.518(6) .
C13 H13 1.0000 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C18 1.500(5) .
C16 C17 1.505(5) .
C16 H16 1.0000 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C30 C31 1.362(4) .
C30 C30 1.388(7) 6_556
C30 H19 0.9500 .
C19 C20 1.385(3) .
C19 C20 1.385(3) 6
C19 H20 0.9500 .
C20 N2 1.344(3) .
C20 C21 1.513(4) .
C21 H22A 0.9800 .
C21 H22B 0.9800 .
C21 H22C 0.9800 .
C31 C30 1.362(4) 2_665
C31 H25 0.9500 .
N1 Nb1 1.963(2) 5_665
N1 Nb1 1.963(2) .
N2 Nb1 2.235(2) .
Nb1 N1 1.963(2) 5_665
Nb1 N2 2.235(2) 6
Nb1 Nb1 2.7778(6) 5_665
