#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:14:32 +0100 (vie 25 de mar de 2016) $
#$Revision: 179805 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/01/7010132.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_7010132
loop_
_publ_author_name
'Humphries, Martin J.'
'Green, Malcolm L. H.'
'Leech, Michael A.'
'Gibson, Vernon C.'
'Jolly, Matthew'
'Williams, David N.'
'Elsegood, Mark R. J.'
'Clegg, William'
_publ_section_title
;
 Niobium η-cyclopentadienyl compounds with imido and amido ligands
 derived from tert-butylamine
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4044
_journal_paper_doi               10.1039/b006333i
_journal_year                    2000
_chemical_formula_sum            'C21 H32 Cl N2 Nb'
_chemical_formula_weight         440.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.165(2)
_cell_length_b                   14.166(4)
_cell_length_c                   16.807(3)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      10.92
_cell_volume                     2166.8(9)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe-Siemens diffractometer'
_diffrn_measurement_method       'ω/θ 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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4430
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.8262
_exptl_absorpt_correction_T_min  0.7761
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.806
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3822
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0561P)²+4.1726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                2970
_reflns_number_total             3822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006333i.txt
_cod_data_source_block           vcg31
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010132
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb Nb 0.24272(3) 0.03642(2) 0.119346(19) 0.01855(13) Uani 1 1 d . . .
Cl1 Cl 0.20624(12) 0.10071(8) -0.01366(6) 0.0352(3) Uani 1 1 d . A .
C1 C 0.3603(6) -0.0943(4) 0.0529(3) 0.0454(13) Uani 1 1 d . A .
H1 H 0.3913 -0.0836 0.0016 0.055 Uiso 1 1 calc R . .
C2 C 0.4426(5) -0.0776(3) 0.1251(4) 0.0456(13) Uani 1 1 d . A .
H2 H 0.5410 -0.0553 0.1325 0.055 Uiso 1 1 calc R . .
C3 C 0.3560(6) -0.0994(3) 0.1859(3) 0.0418(12) Uani 1 1 d . A .
H3 H 0.3840 -0.0924 0.2419 0.050 Uiso 1 1 calc R . .
C4 C 0.2208(6) -0.1334(3) 0.1495(4) 0.0452(13) Uani 1 1 d . A .
H4 H 0.1418 -0.1551 0.1765 0.054 Uiso 1 1 calc R . .
C5 C 0.2223(6) -0.1298(3) 0.0672(3) 0.0443(12) Uani 1 1 d . A .
H5 H 0.1445 -0.1480 0.0277 0.053 Uiso 1 1 calc R . .
N1 N 0.3458(3) 0.1277(2) 0.17443(18) 0.0194(7) Uani 1 1 d . A .
C6 C 0.4497(4) 0.1865(3) 0.2165(2) 0.0186(8) Uani 1 1 d . . .
C7 C 0.5015(4) 0.1679(3) 0.2979(2) 0.0202(8) Uani 1 1 d . A .
C8 C 0.6084(4) 0.2273(3) 0.3363(2) 0.0247(9) Uani 1 1 d . . .
H8 H 0.6450 0.2155 0.3907 0.030 Uiso 1 1 calc R A .
C9 C 0.6621(4) 0.3029(3) 0.2973(2) 0.0284(9) Uani 1 1 d . A .
H9 H 0.7355 0.3423 0.3247 0.034 Uiso 1 1 calc R . .
C10 C 0.6100(4) 0.3216(3) 0.2185(2) 0.0264(9) Uani 1 1 d . . .
H10 H 0.6474 0.3743 0.1925 0.032 Uiso 1 1 calc R A .
C11 C 0.5037(4) 0.2648(3) 0.1766(2) 0.0220(8) Uani 1 1 d . A .
C12 C 0.4486(4) 0.0832(3) 0.3428(2) 0.0240(8) Uani 1 1 d . . .
H12 H 0.3646 0.0537 0.3082 0.036 Uiso 1 1 calc R A .
C13 C 0.5714(5) 0.0092(3) 0.3577(3) 0.0379(11) Uani 1 1 d . A .
H13A H 0.5355 -0.0451 0.3858 0.057 Uiso 1 1 calc R . .
H13B H 0.6561 0.0371 0.3904 0.057 Uiso 1 1 calc R . .
H13C H 0.6008 -0.0115 0.3063 0.057 Uiso 1 1 calc R . .
C14 C 0.3937(5) 0.1126(3) 0.4219(2) 0.0345(10) Uani 1 1 d . A .
H14A H 0.3584 0.0567 0.4483 0.052 Uiso 1 1 calc R . .
H14B H 0.3132 0.1580 0.4110 0.052 Uiso 1 1 calc R . .
H14C H 0.4743 0.1417 0.4569 0.052 Uiso 1 1 calc R . .
C15 C 0.4481(5) 0.2858(3) 0.0899(2) 0.0305(10) Uani 1 1 d . . .
H15 H 0.4165 0.2246 0.0637 0.046 Uiso 1 1 calc R A .
C16 C 0.5642(6) 0.3290(4) 0.0428(3) 0.0492(13) Uani 1 1 d . A .
H16A H 0.6520 0.2889 0.0484 0.074 Uiso 1 1 calc R . .
H16B H 0.5900 0.3921 0.0637 0.074 Uiso 1 1 calc R . .
H16C H 0.5251 0.3335 -0.0139 0.074 Uiso 1 1 calc R . .
C17 C 0.3147(6) 0.3500(5) 0.0840(3) 0.0550(15) Uani 1 1 d . A .
H17A H 0.2780 0.3602 0.0275 0.083 Uiso 1 1 calc R . .
H17B H 0.3423 0.4108 0.1093 0.083 Uiso 1 1 calc R . .
H17C H 0.2377 0.3206 0.1114 0.083 Uiso 1 1 calc R . .
N2 N 0.0473(4) 0.0466(3) 0.1547(2) 0.0242(9) Uani 0.916(4) 1 d PU A 1
H2A H -0.0071 -0.0028 0.1395 0.029 Uiso 0.916(4) 1 calc PR A 1
Cl2X Cl 0.1236(10) 0.1154(7) 0.1608(5) 0.011(3) Uiso 0.084(4) 1 d PU A 2
C18 C -0.0344(4) 0.1143(3) 0.1997(3) 0.0294(9) Uani 1 1 d U A 1
C19 C -0.1964(5) 0.0894(4) 0.1851(3) 0.0401(12) Uani 1 1 d . A 1
H19A H -0.2299 0.0932 0.1276 0.060 Uiso 1 1 calc R A 1
H19B H -0.2528 0.1338 0.2141 0.060 Uiso 1 1 calc R A 1
H19C H -0.2112 0.0251 0.2041 0.060 Uiso 1 1 calc R A 1
C20 C 0.0174(7) 0.1080(6) 0.2881(3) 0.084(3) Uani 1 1 d . A 1
H20A H 0.1232 0.1207 0.2972 0.126 Uiso 1 1 calc R A 1
H20B H -0.0021 0.0445 0.3075 0.126 Uiso 1 1 calc R A 1
H20C H -0.0351 0.1546 0.3171 0.126 Uiso 1 1 calc R A 1
C21 C -0.0114(6) 0.2132(4) 0.1696(4) 0.0651(18) Uani 1 1 d . A 1
H21A H -0.0714 0.2576 0.1964 0.098 Uiso 1 1 calc R A 1
H21B H -0.0403 0.2157 0.1116 0.098 Uiso 1 1 calc R A 1
H21C H 0.0925 0.2304 0.1813 0.098 Uiso 1 1 calc R A 1
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
Cl2X Nb N1 69.6(3) . . ?
Cl2X Nb N2 37.1(3) . . ?
N1 Nb N2 103.62(14) . . ?
Cl2X Nb C3 125.4(3) . . ?
N1 Nb C3 99.49(16) . . ?
N2 Nb C3 106.20(17) . . ?
Cl2X Nb Cl1 95.9(3) . . ?
N1 Nb Cl1 102.36(10) . . ?
N2 Nb Cl1 102.85(12) . . ?
C3 Nb Cl1 138.03(13) . . ?
Cl2X Nb C2 154.6(3) . . ?
N1 Nb C2 96.31(16) . . ?
N2 Nb C2 138.40(16) . . ?
C3 Nb C2 33.67(17) . . ?
Cl1 Nb C2 108.05(14) . . ?
Cl2X Nb C4 117.9(3) . . ?
N1 Nb C4 130.30(17) . . ?
N2 Nb C4 84.85(16) . . ?
C3 Nb C4 33.40(18) . . ?
Cl1 Nb C4 123.67(14) . . ?
C2 Nb C4 54.92(16) . . ?
Cl2X Nb C1 167.5(3) . . ?
N1 Nb C1 122.80(17) . . ?
N2 Nb C1 130.92(17) . . ?
C3 Nb C1 54.76(17) . . ?
Cl1 Nb C1 83.31(13) . . ?
C2 Nb C1 32.43(18) . . ?
C4 Nb C1 54.16(17) . . ?
Cl2X Nb C5 135.1(3) . . ?
N1 Nb C5 150.37(15) . . ?
N2 Nb C5 98.15(16) . . ?
C3 Nb C5 54.64(17) . . ?
Cl1 Nb C5 91.96(13) . . ?
C2 Nb C5 54.33(17) . . ?
C4 Nb C5 32.28(18) . . ?
C1 Nb C5 32.80(17) . . ?
C2 C1 C5 108.8(5) . . ?
C2 C1 Nb 72.2(3) . . ?
C5 C1 Nb 75.1(3) . . ?
C1 C2 C3 107.9(4) . . ?
C1 C2 Nb 75.3(3) . . ?
C3 C2 Nb 71.7(3) . . ?
C2 C3 C4 107.7(5) . . ?
C2 C3 Nb 74.6(3) . . ?
C4 C3 Nb 76.1(3) . . ?
C5 C4 C3 108.1(4) . . ?
C5 C4 Nb 75.5(3) . . ?
C3 C4 Nb 70.5(3) . . ?
C4 C5 C1 107.4(5) . . ?
C4 C5 Nb 72.2(3) . . ?
C1 C5 Nb 72.1(3) . . ?
C6 N1 Nb 168.5(3) . . ?
C6 N1 Cl2X 136.5(4) . . ?
Nb N1 Cl2X 54.5(3) . . ?
N1 C6 C11 119.0(3) . . ?
N1 C6 C7 120.6(3) . . ?
C11 C6 C7 120.4(3) . . ?
C8 C7 C6 118.2(4) . . ?
C8 C7 C12 119.5(3) . . ?
C6 C7 C12 122.2(3) . . ?
C9 C8 C7 121.4(4) . . ?
C8 C9 C10 120.3(4) . . ?
C9 C10 C11 121.1(4) . . ?
C10 C11 C6 118.5(4) . . ?
C10 C11 C15 120.6(4) . . ?
C6 C11 C15 120.8(3) . . ?
C7 C12 C14 111.8(3) . . ?
C7 C12 C13 110.3(3) . . ?
C14 C12 C13 110.7(4) . . ?
C11 C15 C17 111.0(4) . . ?
C11 C15 C16 113.7(4) . . ?
C17 C15 C16 109.3(4) . . ?
C18 N2 Nb 137.7(3) . . ?
Nb Cl2X N1 55.9(3) . . ?
N2 C18 C20 110.3(4) . . ?
N2 C18 C21 109.3(4) . . ?
C20 C18 C21 110.1(5) . . ?
N2 C18 C19 108.2(3) . . ?
C20 C18 C19 109.5(4) . . ?
C21 C18 C19 109.5(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb Cl2X 1.763(9) . ?
Nb N1 1.794(3) . ?
Nb N2 1.958(3) . ?
Nb C3 2.400(5) . ?
Nb Cl1 2.4004(11) . ?
Nb C2 2.436(4) . ?
Nb C4 2.471(5) . ?
Nb C1 2.475(5) . ?
Nb C5 2.512(5) . ?
C1 C2 1.372(8) . ?
C1 C5 1.409(7) . ?
C2 C3 1.401(7) . ?
C3 C4 1.401(7) . ?
C4 C5 1.386(8) . ?
N1 C6 1.393(5) . ?
N1 Cl2X 2.030(10) . ?
C6 C11 1.415(5) . ?
C6 C7 1.418(5) . ?
C7 C8 1.391(5) . ?
C7 C12 1.527(5) . ?
C8 C9 1.377(6) . ?
C9 C10 1.379(6) . ?
C10 C11 1.390(5) . ?
C11 C15 1.516(5) . ?
C12 C14 1.533(6) . ?
C12 C13 1.537(6) . ?
C15 C17 1.518(7) . ?
C15 C16 1.527(6) . ?
N2 C18 1.478(5) . ?
C18 C20 1.508(7) . ?
C18 C21 1.513(7) . ?
C18 C19 1.518(6) . ?
