#------------------------------------------------------------------------------
#$Date: 2019-10-31 06:08:54 +0100 (jue 31 de oct de 2019) $
#$Revision: 220584 $
#$URL: svn://www.crystallography.net/cod/cif/1/55/25/1552542.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_1552542
loop_
_publ_author_name
'Zanchin, Giorgia'
'Bertini, Fabio'
'Vendier, Laure'
'Ricci, Giovanni'
'Lorber, Christian'
'Leone, Giuseppe'
_publ_section_title
;
 Copolymerization of Ethylene with Propylene and Higher α-Olefins
 Catalyzed by (Imido)vanadium(IV) Dichloride Complexes
;
_journal_name_full               'Polymer Chemistry'
_journal_paper_doi               10.1039/C9PY01415B
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C8 H23 Cl2 N3 V'
_chemical_formula_sum            'C8 H23 Cl2 N3 V'
_chemical_formula_weight         283.13
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-09T13:27:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-07-15 deposited with the CCDC.    2019-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.55(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.139(3)
_cell_length_b                   9.122(2)
_cell_length_c                   12.098(2)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1519.5(8)
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.059
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7615
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.189
_diffrn_reflns_theta_min         3.908
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.98
_exptl_absorpt_correction_T_max  0.7490
_exptl_absorpt_correction_T_min  0.3140
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.62(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         4408
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0619P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                2205
_reflns_number_total             4408
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9py01415b2.cif
_cod_data_source_block           cl511
_cod_original_cell_volume        1519.5(7)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1552542
_shelx_shelxl_version_number     2016/4
_publcif_funding_html
;
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
V1 V 0.7254(2) 0.02581(7) 0.8874(3) 0.0501(2) Uani 1 1 d . .
CL1 Cl 0.82520(9) 0.1137(4) 1.11415(12) 0.0693(8) Uani 1 1 d . .
CL2 Cl 0.62569(10) 0.1111(4) 0.66073(13) 0.0730(9) Uani 1 1 d . .
N1 N 0.7281(9) -0.1535(4) 0.8892(11) 0.0758(12) Uani 1 1 d . .
N2 N 0.6079(7) 0.0733(11) 0.9027(9) 0.063(3) Uani 1 1 d . .
H2 H 0.630858 0.038074 0.995831 0.075 Uiso 1 1 calc R U
N3 N 0.8428(7) 0.0681(12) 0.8764(9) 0.070(3) Uani 1 1 d . .
H3 H 0.82096 0.032987 0.783698 0.084 Uiso 1 1 calc R U
C1 C 0.7415(6) -0.3130(5) 0.8895(9) 0.081(2) Uani 1 1 d D U
C2 C 0.6545(8) -0.3733(14) 0.7589(10) 0.162(5) Uani 1 1 d D U
H2A H 0.650217 -0.331865 0.680719 0.242 Uiso 1 1 calc R U
H2B H 0.59594 -0.347489 0.751305 0.242 Uiso 1 1 calc R U
H2C H 0.659962 -0.48021 0.758683 0.242 Uiso 1 1 calc R U
C3 C 0.7558(8) -0.3710(14) 1.0154(10) 0.113(3) Uani 1 1 d D U
H3A H 0.702577 -0.337561 1.018025 0.169 Uiso 1 1 calc R U
H3B H 0.81771 -0.33528 1.097098 0.169 Uiso 1 1 calc R U
H3C H 0.756467 -0.478411 1.013915 0.169 Uiso 1 1 calc R U
C4 C 0.8309(7) -0.3558(8) 0.8944(10) 0.119(2) Uani 1 1 d D U
H4A H 0.890443 -0.327291 0.98353 0.178 Uiso 1 1 calc R U
H4B H 0.827956 -0.305143 0.82053 0.178 Uiso 1 1 calc R U
H4C H 0.831042 -0.461987 0.882294 0.178 Uiso 1 1 calc R U
C5 C 0.5158(9) -0.0132(19) 0.8008(15) 0.116(5) Uani 1 1 d . .
H5A H 0.494113 0.00766 0.706936 0.173 Uiso 1 1 calc R U
H5B H 0.464952 0.015328 0.810253 0.173 Uiso 1 1 calc R U
H5C H 0.529165 -0.118242 0.819544 0.173 Uiso 1 1 calc R U
C6 C 0.5890(12) 0.2331(15) 0.9007(15) 0.107(5) Uani 1 1 d . .
H6A H 0.537017 0.247477 0.911022 0.161 Uiso 1 1 calc R U
H6B H 0.569377 0.27534 0.813022 0.161 Uiso 1 1 calc R U
H6C H 0.648273 0.281711 0.976604 0.161 Uiso 1 1 calc R U
C7 C 0.8616(9) 0.2302(16) 0.8799(11) 0.088(4) Uani 1 1 d . .
H7A H 0.905773 0.246655 0.85487 0.132 Uiso 1 1 calc R U
H7B H 0.891167 0.267987 0.972789 0.132 Uiso 1 1 calc R U
H7C H 0.800117 0.281132 0.814348 0.132 Uiso 1 1 calc R U
C8 C 0.9368(11) 0.0040(19) 0.9737(14) 0.104(4) Uani 1 1 d . .
H8A H 0.968267 0.051987 1.063182 0.156 Uiso 1 1 calc R U
H8B H 0.976844 0.017086 0.941149 0.156 Uiso 1 1 calc R U
H8C H 0.929515 -0.100923 0.982947 0.156 Uiso 1 1 calc R U
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0531(4) 0.0471(3) 0.0464(3) -0.0012(12) 0.0276(3) -0.0003(11)
CL1 0.0622(16) 0.096(2) 0.0483(15) -0.0110(16) 0.0321(12) -0.0107(15)
CL2 0.0656(16) 0.099(3) 0.0527(16) 0.0130(17) 0.0342(13) 0.0278(17)
N1 0.094(3) 0.050(2) 0.0609(19) -0.007(7) 0.034(2) 0.005(7)
N2 0.048(5) 0.084(6) 0.059(6) -0.005(4) 0.034(5) -0.008(4)
N3 0.065(6) 0.096(7) 0.049(6) -0.001(4) 0.034(5) 0.019(5)
C1 0.125(5) 0.043(2) 0.067(2) -0.002(4) 0.053(3) -0.012(4)
C2 0.170(7) 0.078(6) 0.105(4) -0.024(5) 0.011(6) -0.022(6)
C3 0.154(7) 0.076(5) 0.096(4) 0.022(4) 0.067(5) 0.002(5)
C4 0.160(6) 0.054(4) 0.164(7) 0.006(4) 0.108(5) 0.020(4)
C5 0.054(7) 0.172(14) 0.101(9) -0.026(9) 0.035(7) -0.056(8)
C6 0.096(9) 0.096(10) 0.130(11) -0.021(8) 0.068(8) 0.009(8)
C7 0.075(7) 0.125(11) 0.068(6) -0.011(6) 0.045(5) -0.045(7)
C8 0.084(9) 0.161(13) 0.077(8) 0.009(8) 0.053(7) 0.037(9)
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 0 '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'
V V 0.3005 0.5294 '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
N1 V1 N3 99.3(5)
N1 V1 N2 102.6(5)
N3 V1 N2 158.05(16)
N1 V1 CL2 110.1(4)
N3 V1 CL2 85.6(3)
N2 V1 CL2 88.1(3)
N1 V1 CL1 109.4(4)
N3 V1 CL1 87.3(3)
N2 V1 CL1 84.3(3)
CL2 V1 CL1 140.56(5)
C1 N1 V1 172.3(10)
C6 N2 C5 112.6(12)
C6 N2 V1 113.4(9)
C5 N2 V1 113.2(8)
C8 N3 C7 105.0(12)
C8 N3 V1 121.1(8)
C7 N3 V1 111.7(8)
N1 C1 C3 106.5(8)
N1 C1 C2 107.8(9)
C3 C1 C2 113.9(6)
N1 C1 C4 113.5(7)
C3 C1 C4 108.4(6)
C2 C1 C4 106.9(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
V1 N1 1.636(4)
V1 N3 2.129(10)
V1 N2 2.173(9)
V1 CL2 2.338(3)
V1 CL1 2.346(3)
N1 C1 1.473(6)
N2 C6 1.491(14)
N2 C5 1.521(13)
N3 C8 1.437(15)
N3 C7 1.509(16)
C1 C3 1.489(8)
C1 C2 1.489(8)
C1 C4 1.548(8)
