#------------------------------------------------------------------------------
#$Date: 2015-07-03 10:29:35 +0300 (Fri, 03 Jul 2015) $
#$Revision: 139946 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/09/7220998.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_7220998
loop_
_publ_author_name
'Havlik, Ales'
'Lamač, Martin'
'Pinkas, Jiri'
'R°užička, Aleš'
'Horacek, Michal'
_publ_section_title
;
 Mixed Amido-cyclopentadienyl Group 4 Metal Complexes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA07742G
_journal_year                    2015
_chemical_formula_moiety         'C38 H54 Cl2 N4 Zr2'
_chemical_formula_sum            'C38 H54 Cl2 N4 Zr2'
_chemical_formula_weight         820.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                111.082(4)
_cell_angle_beta                 103.324(5)
_cell_angle_gamma                105.615(5)
_cell_formula_units_Z            1
_cell_length_a                   9.3661(7)
_cell_length_b                   10.4020(8)
_cell_length_c                   11.5359(7)
_cell_measurement_reflns_used    20294
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     940.60(13)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20263
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0314
_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)+(0.0327P)²+0.7287P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                3813
_reflns_number_total             4314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra07742g2.cif
_cod_data_source_block           16
_cod_original_cell_volume        940.61(13)
_cod_database_code               7220998
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Zr1 Zr 0.10504(2) 0.65650(2) 0.52188(2) 0.01623(7) Uani 1 1 d .
Cl1 Cl 0.38194(6) 0.69904(7) 0.54357(6) 0.02624(13) Uani 1 1 d .
N1 N -0.0257(2) 0.4548(2) 0.36673(18) 0.0183(4) Uani 1 1 d .
C1 C -0.1073(3) 0.3586(2) 0.2296(2) 0.0183(4) Uani 1 1 d .
C13 C 0.0365(3) 0.8789(2) 0.6170(2) 0.0215(5) Uani 1 1 d .
C6 C -0.2724(3) 0.2818(3) 0.1775(2) 0.0219(5) Uani 1 1 d .
H6 H -0.3295 0.2996 0.2336 0.026 Uiso 1 1 d R
C12 C -0.0889(3) 0.7749(3) 0.4941(2) 0.0225(5) Uani 1 1 d .
C10 C 0.1340(3) 0.8622(2) 0.4487(2) 0.0215(5) Uani 1 1 d .
C14 C 0.1755(3) 0.9316(2) 0.5898(2) 0.0223(5) Uani 1 1 d .
C2 C -0.0235(3) 0.3359(3) 0.1413(2) 0.0205(4) Uani 1 1 d .
C15 C 0.2436(3) 0.8909(3) 0.3769(3) 0.0298(5) Uani 1 1 d .
H15A H 0.2042 0.8077 0.2902 0.036 Uiso 1 1 d R
H15B H 0.3479 0.9034 0.4268 0.036 Uiso 1 1 d R
H15C H 0.2490 0.9800 0.3676 0.036 Uiso 1 1 d R
C18 C 0.0248(4) 0.9320(3) 0.7520(3) 0.0320(6) Uani 1 1 d .
H18A H 0.0142 1.0265 0.7768 0.038 Uiso 1 1 d R
H18B H 0.1193 0.9433 0.8159 0.038 Uiso 1 1 d R
H18C H -0.0664 0.8605 0.7502 0.038 Uiso 1 1 d R
C17 C -0.2585(3) 0.6946(3) 0.4760(3) 0.0321(6) Uani 1 1 d .
H17A H -0.2605 0.6823 0.5543 0.038 Uiso 1 1 d R
H17B H -0.3031 0.5982 0.4000 0.038 Uiso 1 1 d R
H17C H -0.3198 0.7519 0.4623 0.038 Uiso 1 1 d R
C16 C -0.1247(3) 0.6758(3) 0.2431(2) 0.0300(5) Uani 1 1 d .
H16A H -0.1628 0.7377 0.2103 0.036 Uiso 1 1 d R
H16B H -0.2136 0.5918 0.2283 0.036 Uiso 1 1 d R
H16C H -0.0593 0.6410 0.1969 0.036 Uiso 1 1 d R
C3 C -0.1071(3) 0.2343(3) 0.0082(2) 0.0260(5) Uani 1 1 d .
H3 H -0.0526 0.2194 -0.0502 0.031 Uiso 1 1 d R
N2 N 0.2274(3) 0.3793(3) 0.0964(2) 0.0347(5) Uani 1 1 d .
C11 C -0.0287(3) 0.7647(3) 0.3900(2) 0.0226(5) Uani 1 1 d .
C7 C 0.1527(3) 0.4271(3) 0.1928(2) 0.0276(5) Uani 1 1 d .
H7A H 0.1695 0.5311 0.2181 0.033 Uiso 1 1 d R
H7B H 0.2044 0.4202 0.2722 0.033 Uiso 1 1 d R
C19 C 0.3351(3) 1.0451(3) 0.6901(3) 0.0317(6) Uani 1 1 d .
H19A H 0.3411 1.1434 0.7037 0.038 Uiso 1 1 d R
H19B H 0.4164 1.0253 0.6577 0.038 Uiso 1 1 d R
H19C H 0.3505 1.0394 0.7730 0.038 Uiso 1 1 d R
C5 C -0.3530(3) 0.1794(3) 0.0445(3) 0.0290(5) Uani 1 1 d .
H5 H -0.4627 0.1281 0.0125 0.035 Uiso 1 1 d R
C4 C -0.2702(3) 0.1538(3) -0.0404(3) 0.0319(6) Uani 1 1 d .
H4 H -0.3234 0.0832 -0.1293 0.038 Uiso 1 1 d R
C8 C 0.3684(4) 0.5039(5) 0.1214(4) 0.0649(12) Uani 1 1 d .
H8A H 0.4450 0.5393 0.2087 0.078 Uiso 1 1 d R
H8B H 0.3381 0.5833 0.1161 0.078 Uiso 1 1 d R
H8C H 0.4145 0.4709 0.0557 0.078 Uiso 1 1 d R
C9 C 0.2673(4) 0.2544(4) 0.0990(3) 0.0551(9) Uani 1 1 d .
H9A H 0.3417 0.2844 0.1858 0.066 Uiso 1 1 d R
H9B H 0.3138 0.2228 0.0334 0.066 Uiso 1 1 d R
H9C H 0.1722 0.1731 0.0794 0.066 Uiso 1 1 d R
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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.138
0 -1 0 0.107
0 0 -1 0.082
0 0 1 0.007
1 0 -1 0.052
-1 0 1 0.033
-1 0 0 0.067
1 0 0 0.023
0 1 -1 0.166
0 -1 1 0.091
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
N1 Zr1 N1 83.06(8) . 2_566
N1 Zr1 Cl1 105.72(5) . .
N1 Zr1 Cl1 112.97(5) 2_566 .
N1 Zr1 C12 98.04(8) . .
N1 Zr1 C12 101.17(7) 2_566 .
Cl1 Zr1 C12 140.12(6) . .
N1 Zr1 C13 130.70(8) . .
N1 Zr1 C13 98.19(7) 2_566 .
Cl1 Zr1 C13 118.32(6) . .
C12 Zr1 C13 33.03(8) . .
N1 Zr1 C11 87.82(8) . .
N1 Zr1 C11 131.27(8) 2_566 .
Cl1 Zr1 C11 115.59(6) . .
C12 Zr1 C11 33.20(8) . .
C13 Zr1 C11 54.63(8) . .
N1 Zr1 C14 141.78(8) . .
N1 Zr1 C14 124.68(7) 2_566 .
Cl1 Zr1 C14 88.07(6) . .
C12 Zr1 C14 54.68(8) . .
C13 Zr1 C14 32.84(8) . .
C11 Zr1 C14 54.43(8) . .
N1 Zr1 C10 111.17(8) . .
N1 Zr1 C10 152.21(7) 2_566 .
Cl1 Zr1 C10 86.83(6) . .
C12 Zr1 C10 54.49(8) . .
C13 Zr1 C10 54.26(7) . .
C11 Zr1 C10 32.62(7) . .
C14 Zr1 C10 32.70(7) . .
N1 Zr1 Zr1 43.25(5) . 2_566
N1 Zr1 Zr1 39.81(5) 2_566 2_566
Cl1 Zr1 Zr1 116.370(18) . 2_566
C12 Zr1 Zr1 102.94(6) . 2_566
C13 Zr1 Zr1 121.27(6) . 2_566
C11 Zr1 Zr1 115.51(6) . 2_566
C14 Zr1 Zr1 154.08(6) . 2_566
C10 Zr1 Zr1 147.52(5) . 2_566
C1 N1 Zr1 152.80(15) . .
C1 N1 Zr1 109.04(14) . 2_566
Zr1 N1 Zr1 96.94(8) . 2_566
C6 C1 N1 121.0(2) . .
C6 C1 C2 118.4(2) . .
N1 C1 C2 120.7(2) . .
C12 C13 C14 108.2(2) . .
C12 C13 C18 126.5(2) . .
C14 C13 C18 125.2(2) . .
C12 C13 Zr1 72.50(12) . .
C14 C13 Zr1 74.43(12) . .
C18 C13 Zr1 121.68(15) . .
C5 C6 C1 121.6(2) . .
C5 C6 H6 119.2 . .
C1 C6 H6 119.2 . .
C13 C12 C11 108.0(2) . .
C13 C12 C17 126.0(2) . .
C11 C12 C17 125.9(2) . .
C13 C12 Zr1 74.47(13) . .
C11 C12 Zr1 74.39(13) . .
C17 C12 Zr1 119.39(15) . .
C11 C10 C14 108.0(2) . .
C11 C10 C15 126.6(2) . .
C14 C10 C15 125.4(2) . .
C11 C10 Zr1 72.21(13) . .
C14 C10 Zr1 73.02(13) . .
C15 C10 Zr1 121.51(16) . .
C13 C14 C10 107.8(2) . .
C13 C14 C19 126.4(2) . .
C10 C14 C19 125.8(2) . .
C13 C14 Zr1 72.73(12) . .
C10 C14 Zr1 74.28(13) . .
C19 C14 Zr1 120.91(16) . .
C3 C2 C1 118.9(2) . .
C3 C2 C7 121.6(2) . .
C1 C2 C7 119.4(2) . .
C10 C15 H15A 109.4 . .
C10 C15 H15B 109.4 . .
H15A C15 H15B 109.5 . .
C10 C15 H15C 109.6 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C13 C18 H18A 109.4 . .
C13 C18 H18B 109.4 . .
H18A C18 H18B 109.5 . .
C13 C18 H18C 109.6 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C12 C17 H17A 109.4 . .
C12 C17 H17B 109.4 . .
H17A C17 H17B 109.5 . .
C12 C17 H17C 109.6 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C11 C16 H16A 109.6 . .
C11 C16 H16B 109.3 . .
H16A C16 H16B 109.5 . .
C11 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C2 C3 C4 121.8(2) . .
C2 C3 H3 119.2 . .
C4 C3 H3 119.0 . .
C9 N2 C7 110.6(2) . .
C9 N2 C8 111.0(3) . .
C7 N2 C8 110.7(2) . .
C10 C11 C12 108.0(2) . .
C10 C11 C16 126.0(2) . .
C12 C11 C16 125.7(2) . .
C10 C11 Zr1 75.17(13) . .
C12 C11 Zr1 72.42(13) . .
C16 C11 Zr1 122.16(15) . .
N2 C7 C2 113.5(2) . .
N2 C7 H7A 108.9 . .
C2 C7 H7A 108.9 . .
N2 C7 H7B 108.8 . .
C2 C7 H7B 108.8 . .
H7A C7 H7B 107.7 . .
C14 C19 H19A 109.6 . .
C14 C19 H19B 109.3 . .
H19A C19 H19B 109.5 . .
C14 C19 H19C 109.6 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C4 C5 C6 119.8(2) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.0 . .
C5 C4 C3 119.4(2) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.5 . .
N2 C8 H8A 109.6 . .
N2 C8 H8B 109.2 . .
H8A C8 H8B 109.5 . .
N2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N2 C9 H9A 109.7 . .
N2 C9 H9B 109.4 . .
H9A C9 H9B 109.5 . .
N2 C9 H9C 109.3 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 N1 2.0024(19) .
Zr1 N1 2.1427(19) 2_566
Zr1 Cl1 2.4471(6) .
Zr1 C12 2.477(2) .
Zr1 C13 2.503(2) .
Zr1 C11 2.503(2) .
Zr1 C14 2.524(2) .
Zr1 C10 2.541(2) .
Zr1 Zr1 3.1045(5) 2_566
N1 C1 1.407(3) .
N1 Zr1 2.1427(19) 2_566
C1 C6 1.396(3) .
C1 C2 1.416(3) .
C13 C12 1.416(3) .
C13 C14 1.421(3) .
C13 C18 1.496(3) .
C6 C5 1.385(3) .
C6 H6 0.9300 .
C12 C11 1.423(3) .
C12 C17 1.508(3) .
C10 C11 1.417(3) .
C10 C14 1.426(3) .
C10 C15 1.494(3) .
C14 C19 1.496(3) .
C2 C3 1.385(3) .
C2 C7 1.509(3) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C16 C11 1.503(3) .
C16 H16A 0.9600 .
C16 H16B 0.9599 .
C16 H16C 0.9600 .
C3 C4 1.389(4) .
C3 H3 0.9301 .
N2 C9 1.454(4) .
N2 C7 1.456(3) .
N2 C8 1.463(4) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C5 C4 1.380(4) .
C5 H5 0.9300 .
C4 H4 0.9300 .
C8 H8A 0.9600 .
C8 H8B 0.9601 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9601 .
C9 H9C 0.9600 .
