#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/17/1501780.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_1501780
loop_
_publ_author_name
'Theaker, Giles W.'
'Morton, Colin'
'Scott, Peter'
_publ_section_title
;
 Zirconium-Catalyzed Polymerization of a Styrene: Catalyst Reactivation
 Mechanisms Using Alkenes and Dihydrogen
;
_journal_issue                   6
_journal_name_full               Macromolecules
_journal_page_first              1393
_journal_paper_doi               10.1021/ma102835p
_journal_volume                  44
_journal_year                    2011
_chemical_formula_sum            'C36 H40 Cl2 N2 O4 Zr'
_chemical_formula_weight         726.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 93.635(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.2628(8)
_cell_length_b                   8.7389(3)
_cell_length_c                   16.6065(6)
_cell_measurement_reflns_used    7076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.16
_cell_measurement_theta_min      2.90
_cell_volume                     3369.2(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15077
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         2.80
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0301
_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)+(0.0340P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                3328
_reflns_number_total             4122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma102835p_si_002.cif
_cod_data_source_block           gt2
_cod_depositor_comments          'Adding full bibliography for 1501780.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1501780
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'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zr1 Zr 0.0000 -0.29034(2) 0.2500 0.01272(7) Uani 1 2 d S
O1 O -0.05066(4) -0.31495(12) 0.34131(6) 0.0148(2) Uani 1 1 d .
C1 C -0.06666(7) -0.40546(19) 0.40080(9) 0.0146(3) Uani 1 1 d .
Cl2 Cl 0.066112(17) -0.11319(5) 0.32086(2) 0.01932(10) Uani 1 1 d .
C2 C -0.10966(7) -0.3600(2) 0.45269(9) 0.0160(3) Uani 1 1 d .
C3 C -0.12762(7) -0.4709(2) 0.50554(10) 0.0194(4) Uani 1 1 d .
H3A H -0.1578 -0.4461 0.5392 0.023 Uiso 1 1 calc R
C4 C -0.10347(7) -0.6168(2) 0.51165(10) 0.0202(4) Uani 1 1 d .
H4A H -0.1185 -0.6904 0.5468 0.024 Uiso 1 1 calc R
C5 C -0.05805(7) -0.6535(2) 0.46673(10) 0.0189(4) Uani 1 1 d .
H5A H -0.0397 -0.7502 0.4733 0.023 Uiso 1 1 calc R
C6 C -0.03871(7) -0.54791(19) 0.41114(9) 0.0152(3) Uani 1 1 d .
C7 C 0.01195(7) -0.58735(19) 0.37000(9) 0.0155(3) Uani 1 1 d .
H7A H 0.0284 -0.6844 0.3831 0.019 Uiso 1 1 calc R
N1 N 0.03810(5) -0.50747(15) 0.31740(8) 0.0142(3) Uani 1 1 d .
C8 C 0.08809(7) -0.57647(19) 0.28608(9) 0.0146(3) Uani 1 1 d .
C9 C 0.08864(7) -0.7300(2) 0.26305(10) 0.0169(4) Uani 1 1 d .
H9A H 0.0563 -0.7933 0.2713 0.020 Uiso 1 1 calc R
C10 C 0.13597(7) -0.7897(2) 0.22833(10) 0.0202(4) Uani 1 1 d .
H10A H 0.1363 -0.8944 0.2130 0.024 Uiso 1 1 calc R
C11 C 0.18313(7) -0.6978(2) 0.21569(10) 0.0206(4) Uani 1 1 d .
C12 C 0.18393(7) -0.5465(2) 0.24072(10) 0.0194(4) Uani 1 1 d .
H12A H 0.2168 -0.4845 0.2341 0.023 Uiso 1 1 calc R
C13 C 0.13615(7) -0.4864(2) 0.27563(9) 0.0171(4) Uani 1 1 d .
H13A H 0.1364 -0.3825 0.2925 0.020 Uiso 1 1 calc R
O2 O 0.22704(5) -0.76591(15) 0.17687(8) 0.0294(3) Uani 1 1 d .
C14 C 0.26689(8) -0.6664(2) 0.14218(13) 0.0343(5) Uani 1 1 d .
H14A H 0.2901 -0.7247 0.1056 0.052 Uiso 1 1 calc R
H14B H 0.2922 -0.6206 0.1850 0.052 Uiso 1 1 calc R
H14C H 0.2459 -0.5855 0.1119 0.052 Uiso 1 1 calc R
C15 C -0.13504(7) -0.1976(2) 0.44999(10) 0.0181(4) Uani 1 1 d .
C16 C -0.17159(8) -0.1678(2) 0.52238(11) 0.0268(4) Uani 1 1 d .
H16A H -0.1477 -0.1812 0.5726 0.040 Uiso 1 1 calc R
H16B H -0.2038 -0.2403 0.5211 0.040 Uiso 1 1 calc R
H16C H -0.1866 -0.0631 0.5195 0.040 Uiso 1 1 calc R
C17 C -0.17401(7) -0.1779(2) 0.37207(10) 0.0221(4) Uani 1 1 d .
H17A H -0.1510 -0.1913 0.3251 0.033 Uiso 1 1 calc R
H17B H -0.1910 -0.0752 0.3709 0.033 Uiso 1 1 calc R
H17C H -0.2048 -0.2546 0.3707 0.033 Uiso 1 1 calc R
C18 C -0.08739(7) -0.0760(2) 0.45394(11) 0.0241(4) Uani 1 1 d .
H18A H -0.0632 -0.0886 0.5040 0.036 Uiso 1 1 calc R
H18B H -0.1048 0.0262 0.4528 0.036 Uiso 1 1 calc R
H18C H -0.0637 -0.0878 0.4076 0.036 Uiso 1 1 calc 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'
O O 0.0106 0.0060 '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_
_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
O1 Zr1 O1 167.59(6) 2 .
O1 Zr1 N1 76.90(4) 2 2
O1 Zr1 N1 92.98(4) . 2
O1 Zr1 N1 92.98(4) 2 .
O1 Zr1 N1 76.90(4) . .
N1 Zr1 N1 72.17(6) 2 .
O1 Zr1 Cl2 92.90(3) 2 .
O1 Zr1 Cl2 94.99(3) . .
N1 Zr1 Cl2 162.34(3) 2 .
N1 Zr1 Cl2 94.35(3) . .
O1 Zr1 Cl2 94.99(3) 2 2
O1 Zr1 Cl2 92.90(3) . 2
N1 Zr1 Cl2 94.35(3) 2 2
N1 Zr1 Cl2 162.34(3) . 2
Cl2 Zr1 Cl2 100.95(2) . 2
C1 O1 Zr1 146.42(10) . 2
C1 O1 Zr1 146.42(10) . .
O1 C1 C6 117.68(14) . .
O1 C1 C2 121.57(15) . .
C6 C1 C2 120.74(15) . .
C3 C2 C1 116.13(15) . .
C3 C2 C15 122.16(14) . .
C1 C2 C15 121.72(14) . .
C2 C3 C4 123.22(15) . .
C2 C3 H3A 118.4 . .
C4 C3 H3A 118.4 . .
C5 C4 C3 119.70(16) . .
C5 C4 H4A 120.1 . .
C3 C4 H4A 120.1 . .
C4 C5 C6 119.77(16) . .
C4 C5 H5A 120.1 . .
C6 C5 H5A 120.1 . .
C5 C6 C1 119.82(15) . .
C5 C6 C7 117.51(15) . .
C1 C6 C7 122.56(14) . .
N1 C7 C6 128.47(15) . .
N1 C7 H7A 115.8 . .
C6 C7 H7A 115.8 . .
C7 N1 C8 116.25(14) . .
C7 N1 Zr1 125.18(11) . 2
C8 N1 Zr1 117.16(10) . 2
C7 N1 Zr1 125.18(11) . .
C8 N1 Zr1 117.16(10) . .
C13 C8 C9 119.34(15) . .
C13 C8 N1 118.98(15) . .
C9 C8 N1 121.63(15) . .
C10 C9 C8 120.03(16) . .
C10 C9 H9A 120.0 . .
C8 C9 H9A 120.0 . .
C9 C10 C11 120.33(16) . .
C9 C10 H10A 119.8 . .
C11 C10 H10A 119.8 . .
O2 C11 C10 116.00(16) . .
O2 C11 C12 123.79(16) . .
C10 C11 C12 120.21(16) . .
C11 C12 C13 119.34(16) . .
C11 C12 H12A 120.3 . .
C13 C12 H12A 120.3 . .
C8 C13 C12 120.68(16) . .
C8 C13 H13A 119.7 . .
C12 C13 H13A 119.7 . .
C11 O2 C14 116.65(14) . .
O2 C14 H14A 109.5 . .
O2 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
O2 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C18 C15 C2 111.31(13) . .
C18 C15 C16 106.44(14) . .
C2 C15 C16 111.33(14) . .
C18 C15 C17 110.07(14) . .
C2 C15 C17 109.40(13) . .
C16 C15 C17 108.21(14) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Zr1 O1 1.9902(10)
Zr1 N1 2.3480(13)
Zr1 Cl2 2.4325(4)
O1 C1 1.3368(19)
C1 C6 1.410(2)
C1 C2 1.418(2)
C2 C3 1.390(2)
C2 C15 1.537(2)
C3 C4 1.394(2)
C3 H3A 0.9500
C4 C5 1.370(2)
C4 H4A 0.9500
C5 C6 1.399(2)
C5 H5A 0.9500
C6 C7 1.441(2)
C7 N1 1.299(2)
C7 H7A 0.9500
N1 C8 1.436(2)
C8 C13 1.387(2)
C8 C9 1.395(2)
C9 C10 1.378(2)
C9 H9A 0.9500
C10 C11 1.386(2)
C10 H10A 0.9500
C11 O2 1.377(2)
C11 C12 1.386(3)
C12 C13 1.389(2)
C12 H12A 0.9500
C13 H13A 0.9500
O2 C14 1.419(2)
C14 H14A 0.9800
C14 H14B 0.9800
C14 H14C 0.9800
C15 C18 1.534(2)
C15 C16 1.538(2)
C15 C17 1.542(2)
C16 H16A 0.9800
C16 H16B 0.9800
C16 H16C 0.9800
C17 H17A 0.9800
C17 H17B 0.9800
C17 H17C 0.9800
C18 H18A 0.9800
C18 H18B 0.9800
C18 H18C 0.9800
