#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/72/4077202.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_4077202
loop_
_publ_author_name
'Antiñolo, Antonio'
'López-Solera, Isabel'
'Orive, Irache'
'Otero, Antonio'
'Prashar, Sanjiv'
'Rodríguez, Ana M.'
'Villaseñor, Elena'
_publ_section_title
;
 Niobium and Zirconium Complexes Incorporating Asymmetrically
 SubstitutedansaLigands. X-ray Crystal Structures of
 [Me2Si(η5-C5Me4)(η5-C5H3R)]Nb(NtBu)Cl (R = Me,iPr) and
 [Me2Si(η5-C5Me4)(η5-C5H3R)]ZrCl2(R = H, Me)
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              71
_journal_paper_doi               10.1021/om0006662
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C8 H11 Cl Si0.5 Zr0.5'
_chemical_formula_weight         202.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.1068(7)
_cell_length_b                   13.8030(10)
_cell_length_c                   12.402(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    250(2)
_cell_volume                     1730.1(5)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2133
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0396
_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)+(0.0319P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                1308
_reflns_number_total             2133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0006662.cif
_cod_data_source_block           13
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C8 H11 Cl Si0.50 Zr0.50'
_cod_database_code               4077202
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.09866(6) 0.2500 0.45696(4) 0.02971(17) Uani 1 2 d S
Cl1 Cl 0.10557(14) 0.10950(9) 0.33624(9) 0.0575(4) Uani 1 1 d .
Si1 Si 0.08440(17) 0.2500 0.71723(13) 0.0360(4) Uani 1 2 d S
C1 C 0.2232(5) 0.2500 0.6201(4) 0.0261(13) Uani 1 2 d S
C2 C 0.2694(4) 0.3355(3) 0.5637(3) 0.0274(9) Uani 1 1 d .
C3 C 0.3448(4) 0.3026(3) 0.4779(3) 0.0361(11) Uani 1 1 d .
C4 C 0.2500(4) 0.4442(3) 0.5915(4) 0.0424(11) Uani 1 1 d .
H4A H 0.1925 0.4500 0.6527 0.064 Uiso 1 1 calc .
H4B H 0.2114 0.4769 0.5309 0.064 Uiso 1 1 calc .
H4C H 0.3342 0.4728 0.6080 0.064 Uiso 1 1 calc .
C5 C 0.4223(5) 0.3667(4) 0.4048(4) 0.0623(15) Uani 1 1 d .
H5A H 0.4684 0.3279 0.3527 0.093 Uiso 1 1 calc .
H5B H 0.4852 0.4032 0.4463 0.093 Uiso 1 1 calc .
H5C H 0.3635 0.4104 0.3684 0.093 Uiso 1 1 calc .
C6 C -0.0466(6) 0.2500 0.6134(5) 0.0369(15) Uani 1 2 d S
C7 C -0.0837(4) 0.1659(3) 0.5538(4) 0.0421(11) Uani 1 1 d .
H7 H -0.0694 0.1018 0.5738 0.050 Uiso 1 1 calc .
C8 C -0.1451(4) 0.1978(3) 0.4604(4) 0.0442(11) Uani 1 1 d .
H8 H -0.1803 0.1584 0.4067 0.053 Uiso 1 1 calc .
C9 C 0.0815(5) 0.3626(4) 0.8020(4) 0.0598(15) Uani 1 1 d .
H9A H 0.0080 0.3599 0.8509 0.090 Uiso 1 1 calc .
H9B H 0.0726 0.4183 0.7562 0.090 Uiso 1 1 calc .
H9C H 0.1624 0.3673 0.8422 0.090 Uiso 1 1 calc .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
C1 Zr1 C6 68.99(19) . .
C1 Zr1 Cl1 120.24(6) . 7_565
C6 Zr1 Cl1 120.29(7) . 7_565
C1 Zr1 Cl1 120.24(6) . .
C6 Zr1 Cl1 120.29(7) . .
Cl1 Zr1 Cl1 104.60(7) 7_565 .
C1 Zr1 C2 34.64(11) . .
C6 Zr1 C2 89.67(16) . .
Cl1 Zr1 C2 85.97(9) 7_565 .
Cl1 Zr1 C2 133.17(10) . .
C1 Zr1 C2 34.64(11) . 7_565
C6 Zr1 C2 89.67(16) . 7_565
Cl1 Zr1 C2 133.17(10) 7_565 7_565
Cl1 Zr1 C2 85.97(9) . 7_565
C2 Zr1 C2 56.94(18) . 7_565
C1 Zr1 C7 88.93(16) . 7_565
C6 Zr1 C7 33.68(12) . 7_565
Cl1 Zr1 C7 86.95(11) 7_565 7_565
Cl1 Zr1 C7 133.26(11) . 7_565
C2 Zr1 C7 92.06(13) . 7_565
C2 Zr1 C7 118.75(13) 7_565 7_565
C1 Zr1 C7 88.93(16) . .
C6 Zr1 C7 33.68(12) . .
Cl1 Zr1 C7 133.26(11) 7_565 .
Cl1 Zr1 C7 86.95(11) . .
C2 Zr1 C7 118.75(13) . .
C2 Zr1 C7 92.06(13) 7_565 .
C7 Zr1 C7 55.6(2) 7_565 .
C1 Zr1 C8 119.52(17) . 7_565
C6 Zr1 C8 53.69(17) . 7_565
Cl1 Zr1 C8 79.35(11) 7_565 7_565
Cl1 Zr1 C8 105.05(11) . 7_565
C2 Zr1 C8 121.78(14) . 7_565
C2 Zr1 C8 142.60(14) 7_565 7_565
C7 Zr1 C8 31.78(14) 7_565 7_565
C7 Zr1 C8 53.99(14) . 7_565
C1 Zr1 C8 119.52(17) . .
C6 Zr1 C8 53.69(17) . .
Cl1 Zr1 C8 105.05(11) 7_565 .
Cl1 Zr1 C8 79.35(11) . .
C2 Zr1 C8 142.59(14) . .
C2 Zr1 C8 121.78(14) 7_565 .
C7 Zr1 C8 53.99(14) 7_565 .
C7 Zr1 C8 31.78(14) . .
C8 Zr1 C8 32.6(2) 7_565 .
C1 Zr1 C3 53.92(15) . .
C6 Zr1 C3 119.80(16) . .
Cl1 Zr1 C3 79.22(10) 7_565 .
Cl1 Zr1 C3 104.72(10) . .
C2 Zr1 C3 31.53(12) . .
C2 Zr1 C3 54.08(13) 7_565 .
C7 Zr1 C3 121.98(13) 7_565 .
C7 Zr1 C3 142.17(13) . .
C8 Zr1 C3 146.79(13) 7_565 .
C8 Zr1 C3 173.34(13) . .
C1 Zr1 C3 53.92(15) . 7_565
C6 Zr1 C3 119.80(16) . 7_565
Cl1 Zr1 C3 104.72(11) 7_565 7_565
Cl1 Zr1 C3 79.22(10) . 7_565
C2 Zr1 C3 54.08(13) . 7_565
C2 Zr1 C3 31.53(12) 7_565 7_565
C7 Zr1 C3 142.17(13) 7_565 7_565
C7 Zr1 C3 121.98(13) . 7_565
C8 Zr1 C3 173.34(13) 7_565 7_565
C8 Zr1 C3 146.79(13) . 7_565
C3 Zr1 C3 32.4(2) . 7_565
C6 Si1 C1 95.2(2) . .
C6 Si1 C9 112.28(19) . .
C1 Si1 C9 112.13(18) . .
C6 Si1 C9 112.28(19) . 7_565
C1 Si1 C9 112.13(18) . 7_565
C9 Si1 C9 111.8(3) . 7_565
C6 Si1 Zr1 48.37(19) . .
C1 Si1 Zr1 46.80(17) . .
C9 Si1 Zr1 124.07(17) . .
C9 Si1 Zr1 124.07(17) 7_565 .
C2 C1 C2 109.0(5) . 7_565
C2 C1 Si1 124.0(2) . .
C2 C1 Si1 124.0(2) 7_565 .
C2 C1 Zr1 76.1(3) . .
C2 C1 Zr1 76.1(3) 7_565 .
Si1 C1 Zr1 98.8(2) . .
C3 C2 C1 106.4(4) . .
C3 C2 C4 123.8(4) . .
C1 C2 C4 129.7(4) . .
C3 C2 Zr1 79.4(2) . .
C1 C2 Zr1 69.2(3) . .
C4 C2 Zr1 119.4(3) . .
C2 C3 C3 109.1(2) . 7_565
C2 C3 C5 124.2(4) . .
C3 C3 C5 126.5(3) 7_565 .
C2 C3 Zr1 69.1(2) . .
C3 C3 Zr1 73.82(10) 7_565 .
C5 C3 Zr1 127.4(3) . .
C7 C6 C7 108.9(5) . 7_565
C7 C6 Si1 123.4(3) . .
C7 C6 Si1 123.4(3) 7_565 .
C7 C6 Zr1 75.2(3) . .
C7 C6 Zr1 75.2(3) 7_565 .
Si1 C6 Zr1 97.1(2) . .
C8 C7 C6 107.0(4) . .
C8 C7 Zr1 77.3(3) . .
C6 C7 Zr1 71.1(3) . .
C7 C8 C8 108.5(3) . 7_565
C7 C8 Zr1 70.9(2) . .
C8 C8 Zr1 73.69(10) 7_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 C1 2.383(5) .
Zr1 C6 2.434(6) .
Zr1 Cl1 2.4510(12) 7_565
Zr1 Cl1 2.4511(12) .
Zr1 C2 2.475(4) .
Zr1 C2 2.475(4) 7_565
Zr1 C7 2.487(4) 7_565
Zr1 C7 2.487(4) .
Zr1 C8 2.567(4) 7_565
Zr1 C8 2.567(4) .
Zr1 C3 2.605(4) .
Zr1 C3 2.605(4) 7_565
Si1 C6 1.847(7) .
Si1 C1 1.849(6) .
Si1 C9 1.877(5) .
Si1 C9 1.877(5) 7_565
C1 C2 1.449(5) .
C1 C2 1.449(5) 7_565
C2 C3 1.386(5) .
C2 C4 1.552(6) .
C3 C3 1.452(9) 7_565
C3 C5 1.489(6) .
C6 C7 1.426(6) .
C6 C7 1.426(6) 7_565
C7 C8 1.386(6) .
C8 C8 1.442(9) 7_565
