#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/06/2220674.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2220674
loop_
_publ_author_name
'Esterhuysen, Catharine'
'Retief, Lizette'
'Kruger, Gert J.'
'Cronje, Stephanie'
'Raubenheimer, Helgard G.'
_publ_section_title
Pentacarbonyl-2κ⁵C-chlorido-1κCl-bis[1(η⁵)-cyclopentadienyl](μ-1-oxidoethylene-1:2κ²O:C)chromium(0)zirconium(IV)
_journal_coeditor_code           AT2691
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m125
_journal_paper_doi               10.1107/S1600536808042621
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Cr Zr (C5 H5)2 (C2 H3 O) Cl (C O)5]'
_chemical_formula_moiety         'C17 H13 Cl Cr O6 Zr'
_chemical_formula_sum            'C17 H13 Cl Cr O6 Zr'
_chemical_formula_weight         491.94
_chemical_name_systematic
;
Pentacarbonyl-2κ⁵C-chlorido-1\kCl-bis[1(η⁵)-cyclopentadienyl](μ-1-
oxidoethylene-1:2κ²O:C)chromiumzirconium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.826(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7395(7)
_cell_length_b                   12.1117(6)
_cell_length_c                   12.7859(7)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      2
_cell_volume                     1937.71(18)
_computing_cell_refinement       'PWPC (Gomm, 1998)'
_computing_data_collection       'PWPC (Gomm, 1998)'
_computing_data_reduction        'Xtal3.4 (Hall et al.,  1995)'
_computing_molecular_graphics
'X-SEED (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Philips PW1100'
_diffrn_measurement_method       ω--2θ
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3423
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,  1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.584
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.053P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                2332
_reflns_number_total             3423
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2691.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2220674
_cod_database_fobs_code          2220674
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr1 0.67690(3) 0.45977(3) 0.79870(3) 0.03838(16) Uani d . 1 . .
Cr Cr2 0.82371(6) 0.82936(6) 0.79664(6) 0.0441(2) Uani d . 1 . .
Cl Cl1 0.51592(14) 0.56328(16) 0.80604(18) 0.1054(7) Uani d . 1 . .
O O1 0.6062(3) 0.7896(4) 0.6561(3) 0.0785(12) Uani d . 1 . .
O O2 0.7878(4) 1.0760(3) 0.7936(4) 0.1005(16) Uani d . 1 . .
O O3 0.7167(4) 0.7914(4) 0.9852(4) 0.1065(17) Uani d . 1 . .
O O4 0.9358(4) 0.8437(4) 0.6086(4) 0.0886(14) Uani d . 1 . .
O O5 1.0309(4) 0.8682(5) 0.9517(4) 0.1162(19) Uani d . 1 . .
O O6 0.7769(3) 0.5916(3) 0.8006(3) 0.0532(9) Uani d . 1 . .
C C1 0.6880(4) 0.8052(4) 0.7069(4) 0.0492(12) Uani d . 1 . .
C C2 0.8007(5) 0.9823(5) 0.7944(4) 0.0631(15) Uani d . 1 . .
C C3 0.7572(5) 0.8072(5) 0.9152(5) 0.0627(15) Uani d . 1 . .
C C4 0.8933(4) 0.8394(4) 0.6786(5) 0.0566(13) Uani d . 1 . .
C C5 0.9534(5) 0.8515(5) 0.8931(5) 0.0689(16) Uani d . 1 . .
C C6 0.8496(4) 0.6625(4) 0.7962(4) 0.0449(11) Uani d . 1 . .
C C7 0.9547(4) 0.6101(5) 0.7899(6) 0.086(2) Uani d . 1 . .
H H7A 1.0080 0.6678 0.7871 0.129 Uiso calc R 1 . .
H H7B 0.9469 0.5645 0.7256 0.129 Uiso calc R 1 . .
H H7C 0.9780 0.5639 0.8528 0.129 Uiso calc R 1 . .
C C8 0.8066(5) 0.4232(6) 0.9667(5) 0.0733(18) Uani d . 1 . .
H H8 0.8737 0.4599 0.9772 0.088 Uiso calc R 1 . .
C C9 0.7144(6) 0.4611(5) 0.9977(4) 0.0769(19) Uani d . 1 . .
H H9 0.7065 0.5287 1.0332 0.092 Uiso calc R 1 . .
C C10 0.6349(5) 0.3814(6) 0.9672(4) 0.0758(18) Uani d . 1 . .
H H10 0.5635 0.3850 0.9787 0.091 Uiso calc R 1 . .
C C11 0.6779(6) 0.2982(5) 0.9184(5) 0.0762(19) Uani d . 1 . .
H H11 0.6414 0.2335 0.8893 0.091 Uiso calc R 1 . .
C C12 0.7831(6) 0.3228(5) 0.9179(5) 0.0711(17) Uani d . 1 . .
H H12 0.8315 0.2779 0.8887 0.085 Uiso calc R 1 . .
C C13 0.7269(6) 0.4442(6) 0.6179(5) 0.081(2) Uani d . 1 . .
H H13 0.7843 0.4867 0.6012 0.097 Uiso calc R 1 . .
C C14 0.6228(6) 0.4758(6) 0.6006(5) 0.084(2) Uani d . 1 . .
H H14 0.5943 0.5445 0.5727 0.100 Uiso calc R 1 . .
C C15 0.5653(7) 0.3857(10) 0.6326(6) 0.119(3) Uani d . 1 . .
H H15 0.4901 0.3814 0.6282 0.142 Uiso calc R 1 . .
C C16 0.6386(11) 0.3060(7) 0.6711(6) 0.124(4) Uani d . 1 . .
H H16 0.6228 0.2365 0.6989 0.149 Uiso calc R 1 . .
C C17 0.7361(9) 0.3420(7) 0.6632(5) 0.106(3) Uani d . 1 . .
H H17 0.8011 0.3027 0.6854 0.127 Uiso calc R 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'
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'
Cr Cr 0.3209 0.6236 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O6 Zr1 Cl1 . . 97.24(10) ?
O6 Zr1 C16 . . 130.2(3) ?
Cl1 Zr1 C16 . . 110.7(3) ?
O6 Zr1 C17 . . 100.8(3) ?
Cl1 Zr1 C17 . . 134.4(2) ?
C16 Zr1 C17 . . 31.5(3) ?
O6 Zr1 C12 . . 104.4(2) ?
Cl1 Zr1 C12 . . 133.79(17) ?
C16 Zr1 C12 . . 85.4(3) ?
C17 Zr1 C12 . . 80.9(2) ?
O6 Zr1 C11 . . 132.73(19) ?
Cl1 Zr1 C11 . . 106.9(2) ?
C16 Zr1 C11 . . 77.9(3) ?
C17 Zr1 C11 . . 90.6(3) ?
C12 Zr1 C11 . . 32.2(2) ?
O6 Zr1 C15 . . 123.2(2) ?
Cl1 Zr1 C15 . . 82.4(3) ?
C16 Zr1 C15 . . 32.1(3) ?
C17 Zr1 C15 . . 52.7(3) ?
C12 Zr1 C15 . . 116.3(3) ?
C11 Zr1 C15 . . 100.2(3) ?
O6 Zr1 C8 . . 79.46(18) ?
Cl1 Zr1 C8 . . 119.22(18) ?
C16 Zr1 C8 . . 117.0(3) ?
C17 Zr1 C8 . . 105.2(3) ?
C12 Zr1 C8 . . 32.1(2) ?
C11 Zr1 C8 . . 53.3(2) ?
C15 Zr1 C8 . . 148.3(3) ?
O6 Zr1 C9 . . 89.1(2) ?
Cl1 Zr1 C9 . . 87.62(17) ?
C16 Zr1 C9 . . 130.9(3) ?
C17 Zr1 C9 . . 133.9(2) ?
C12 Zr1 C9 . . 53.1(2) ?
C11 Zr1 C9 . . 53.1(2) ?
C15 Zr1 C9 . . 147.1(3) ?
C8 Zr1 C9 . . 32.3(2) ?
O6 Zr1 C10 . . 121.38(19) ?
Cl1 Zr1 C10 . . 81.00(17) ?
C16 Zr1 C10 . . 103.6(3) ?
C17 Zr1 C10 . . 121.9(3) ?
C12 Zr1 C10 . . 52.9(2) ?
C11 Zr1 C10 . . 31.5(2) ?
C15 Zr1 C10 . . 114.7(3) ?
C8 Zr1 C10 . . 53.5(2) ?
C9 Zr1 C10 . . 32.5(2) ?
O6 Zr1 C14 . . 90.23(19) ?
Cl1 Zr1 C14 . . 85.7(2) ?
C16 Zr1 C14 . . 53.6(3) ?
C17 Zr1 C14 . . 52.9(3) ?
C12 Zr1 C14 . . 133.6(2) ?
C11 Zr1 C14 . . 130.8(2) ?
C15 Zr1 C14 . . 33.0(2) ?
C8 Zr1 C14 . . 153.9(3) ?
C9 Zr1 C14 . . 173.1(2) ?
C10 Zr1 C14 . . 146.9(2) ?
O6 Zr1 C13 . . 78.71(18) ?
Cl1 Zr1 C13 . . 115.91(19) ?
C16 Zr1 C13 . . 52.3(3) ?
C17 Zr1 C13 . . 31.7(2) ?
C12 Zr1 C13 . . 108.2(2) ?
C11 Zr1 C13 . . 122.3(2) ?
C15 Zr1 C13 . . 52.6(3) ?
C8 Zr1 C13 . . 122.5(3) ?
C9 Zr1 C13 . . 154.5(3) ?
C10 Zr1 C13 . . 153.4(2) ?
C14 Zr1 C13 . . 31.4(2) ?
C2 Cr2 C5 . . 89.1(2) ?
C2 Cr2 C3 . . 93.4(2) ?
C5 Cr2 C3 . . 88.0(3) ?
C2 Cr2 C4 . . 91.1(2) ?
C5 Cr2 C4 . . 91.6(3) ?
C3 Cr2 C4 . . 175.4(2) ?
C2 Cr2 C1 . . 91.2(2) ?
C5 Cr2 C1 . . 176.2(2) ?
C3 Cr2 C1 . . 88.2(2) ?
C4 Cr2 C1 . . 92.2(2) ?
C2 Cr2 C6 . . 178.9(2) ?
C5 Cr2 C6 . . 91.2(2) ?
C3 Cr2 C6 . . 87.6(2) ?
C4 Cr2 C6 . . 87.8(2) ?
C1 Cr2 C6 . . 88.58(19) ?
C6 O6 Zr1 . . 170.5(3) y
O1 C1 Cr2 . . 178.0(5) ?
O2 C2 Cr2 . . 179.2(6) ?
O3 C3 Cr2 . . 178.3(6) ?
O4 C4 Cr2 . . 178.7(5) ?
O5 C5 Cr2 . . 177.9(6) ?
O6 C6 C7 . . 112.5(4) ?
O6 C6 Cr2 . . 123.2(3) ?
C7 C6 Cr2 . . 124.3(4) ?
C6 C7 H7A . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C6 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C12 C8 C9 . . 107.3(6) ?
C12 C8 Zr1 . . 73.3(3) ?
C9 C8 Zr1 . . 74.2(3) ?
C12 C8 H8 . . 126.3 ?
C9 C8 H8 . . 126.3 ?
Zr1 C8 H8 . . 118.2 ?
C8 C9 C10 . . 107.4(6) ?
C8 C9 Zr1 . . 73.5(3) ?
C10 C9 Zr1 . . 73.9(3) ?
C8 C9 H9 . . 126.3 ?
C10 C9 H9 . . 126.3 ?
Zr1 C9 H9 . . 118.3 ?
C11 C10 C9 . . 107.9(6) ?
C11 C10 Zr1 . . 73.4(3) ?
C9 C10 Zr1 . . 73.6(3) ?
C11 C10 H10 . . 126.0 ?
C9 C10 H10 . . 126.0 ?
Zr1 C10 H10 . . 118.8 ?
C10 C11 C12 . . 108.6(6) ?
C10 C11 Zr1 . . 75.1(3) ?
C12 C11 Zr1 . . 73.6(3) ?
C10 C11 H11 . . 125.7 ?
C12 C11 H11 . . 125.7 ?
Zr1 C11 H11 . . 117.6 ?
C8 C12 C11 . . 108.7(6) ?
C8 C12 Zr1 . . 74.6(3) ?
C11 C12 Zr1 . . 74.2(3) ?
C8 C12 H12 . . 125.7 ?
C11 C12 H12 . . 125.7 ?
Zr1 C12 H12 . . 117.5 ?
C14 C13 C17 . . 109.2(7) ?
C14 C13 Zr1 . . 73.8(4) ?
C17 C13 Zr1 . . 72.2(4) ?
C14 C13 H13 . . 125.4 ?
C17 C13 H13 . . 125.4 ?
Zr1 C13 H13 . . 120.3 ?
C13 C14 C15 . . 106.2(7) ?
C13 C14 Zr1 . . 74.9(3) ?
C15 C14 Zr1 . . 73.0(3) ?
C13 C14 H14 . . 126.9 ?
C15 C14 H14 . . 126.9 ?
Zr1 C14 H14 . . 117.5 ?
C16 C15 C14 . . 107.0(8) ?
C16 C15 Zr1 . . 72.9(4) ?
C14 C15 Zr1 . . 74.1(4) ?
C16 C15 H15 . . 126.5 ?
C14 C15 H15 . . 126.5 ?
Zr1 C15 H15 . . 118.6 ?
C17 C16 C15 . . 108.9(8) ?
C17 C16 Zr1 . . 74.5(4) ?
C15 C16 Zr1 . . 75.0(5) ?
C17 C16 H16 . . 125.5 ?
C15 C16 H16 . . 125.5 ?
Zr1 C16 H16 . . 116.8 ?
C16 C17 C13 . . 108.7(9) ?
C16 C17 Zr1 . . 74.0(5) ?
C13 C17 Zr1 . . 76.1(4) ?
C16 C17 H17 . . 125.7 ?
C13 C17 H17 . . 125.6 ?
Zr1 C17 H17 . . 116.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 O6 . 2.041(3) y
Zr1 Cl1 . 2.4205(16) ?
Zr1 C16 . 2.463(7) ?
Zr1 C17 . 2.470(6) ?
Zr1 C12 . 2.476(5) ?
Zr1 C11 . 2.483(5) ?
Zr1 C15 . 2.490(6) ?
Zr1 C8 . 2.492(5) ?
Zr1 C9 . 2.500(5) ?
Zr1 C10 . 2.503(5) ?
Zr1 C14 . 2.504(6) ?
Zr1 C13 . 2.517(6) ?
Cr2 C2 . 1.875(6) ?
Cr2 C5 . 1.885(6) ?
Cr2 C3 . 1.889(6) ?
Cr2 C4 . 1.892(6) ?
Cr2 C1 . 1.910(6) ?
Cr2 C6 . 2.048(5) ?
O1 C1 . 1.135(6) ?
O2 C2 . 1.146(6) ?
O3 C3 . 1.130(6) ?
O4 C4 . 1.131(6) ?
O5 C5 . 1.141(7) ?
O6 C6 . 1.271(5) y
C6 C7 . 1.498(7) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 C12 . 1.373(8) ?
C8 C9 . 1.387(9) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.400(9) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.354(9) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.374(9) ?
C11 H11 . 0.9500 ?
C12 H12 . 0.9500 ?
C13 C14 . 1.358(9) ?
C13 C17 . 1.362(9) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.417(10) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.368(13) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.338(12) ?
C16 H16 . 0.9500 ?
C17 H17 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C16 H16 Cl1 2_646 0.95 2.74 3.581(8) 148.5
