#------------------------------------------------------------------------------
#$Date: 2025-08-20 15:06:16 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301830 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/72/4077203.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_4077203
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            'C8.5 H11.5 Cl Si0.5 Zr0.5'
_chemical_formula_weight         208.78
_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                   10.626(8)
_cell_length_b                   13.839(3)
_cell_length_c                   12.470(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    250(2)
_cell_volume                     1833.8(19)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.4883
_diffrn_reflns_av_sigmaI/netI    0.2850
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2993
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0011(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.3153
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0700P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.2625
_reflns_number_gt                490
_reflns_number_total             2293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0006662.cif
_cod_data_source_block           14
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C8.50 H11.50 Cl Si0.50 Zr0.50'
_cod_database_code               4077203
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 0.3776(2) 0.2500 0.46809(15) 0.0616(8) Uani 1 2 d S
Cl1 Cl 0.3800(5) 0.1153(4) 0.3451(3) 0.1141(18) Uani 1 1 d .
Si1 Si 0.3760(11) 0.2500 0.7344(5) 0.116(3) Uani 1 2 d S
C1 C 0.249(2) 0.2500 0.6246(18) 0.065(7) Uiso 1 2 d S
C2 C 0.2124(13) 0.1684(14) 0.5751(13) 0.081(6) Uani 1 1 d .
C3 C 0.1453(13) 0.2001(13) 0.4763(12) 0.106(9) Uani 1 1 d .
C4 C 0.226(2) 0.062(2) 0.5948(18) 0.171(11) Uani 1 1 d .
H4A H 0.1889 0.0270 0.5361 0.256 Uiso 1 1 calc .
H4B H 0.1831 0.0453 0.6601 0.256 Uiso 1 1 calc .
H4C H 0.3131 0.0458 0.6007 0.256 Uiso 1 1 calc .
C5 C 0.0760(14) 0.1400(19) 0.3988(14) 0.163(11) Uani 1 1 d .
H5A H 0.0950 0.0731 0.4112 0.244 Uiso 1 1 calc .
H5B H 0.1006 0.1573 0.3273 0.244 Uiso 1 1 calc .
H5C H -0.0128 0.1504 0.4074 0.244 Uiso 1 1 calc .
C6 C 0.505(2) 0.2500 0.6345(14) 0.088(11) Uani 1 2 d S
C7 C 0.5424(16) 0.1722(15) 0.5707(13) 0.089(7) Uani 1 1 d .
H7 H 0.5242 0.1080 0.5863 0.107 Uiso 1 1 calc .
C8 C 0.6066(15) 0.2008(13) 0.4850(11) 0.093(8) Uani 1 1 d .
C9 C 0.686(4) 0.166(4) 0.391(4) 0.23(3) Uani 0.50 1 d P
H9A H 0.6776 0.0976 0.3833 0.352 Uiso 0.50 1 calc P
H9B H 0.7725 0.1825 0.4029 0.352 Uiso 0.50 1 calc P
H9C H 0.6573 0.1972 0.3261 0.352 Uiso 0.50 1 calc P
C10 C 0.3816(19) 0.357(2) 0.8170(12) 0.203(13) Uani 1 1 d .
H10A H 0.3790 0.4130 0.7722 0.304 Uiso 1 1 calc .
H10B H 0.4580 0.3567 0.8581 0.304 Uiso 1 1 calc .
H10C H 0.3106 0.3570 0.8647 0.304 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 Cl1 121.8(3) . 7_565
C1 Zr1 Cl1 121.8(3) . .
Cl1 Zr1 Cl1 101.1(2) 7_565 .
C1 Zr1 C7 88.9(6) . .
Cl1 Zr1 C7 132.2(5) 7_565 .
Cl1 Zr1 C7 89.1(5) . .
C1 Zr1 C7 88.9(7) . 7_565
Cl1 Zr1 C7 89.1(5) 7_565 7_565
Cl1 Zr1 C7 132.2(5) . 7_565
C7 Zr1 C7 52.8(9) . 7_565
C1 Zr1 C6 68.2(7) . .
Cl1 Zr1 C6 121.7(3) 7_565 .
Cl1 Zr1 C6 121.7(3) . .
C7 Zr1 C6 33.0(5) . .
C7 Zr1 C6 33.0(5) 7_565 .
C1 Zr1 C2 32.1(4) . 7_565
Cl1 Zr1 C2 89.9(4) 7_565 7_565
Cl1 Zr1 C2 134.6(5) . 7_565
C7 Zr1 C2 115.5(5) . 7_565
C7 Zr1 C2 91.4(5) 7_565 7_565
C6 Zr1 C2 86.4(6) . 7_565
C1 Zr1 C2 32.1(4) . .
Cl1 Zr1 C2 134.6(5) 7_565 .
Cl1 Zr1 C2 89.9(5) . .
C7 Zr1 C2 91.4(5) . .
C7 Zr1 C2 115.5(5) 7_565 .
C6 Zr1 C2 86.4(6) . .
C2 Zr1 C2 54.2(9) 7_565 .
C1 Zr1 C8 118.8(6) . 7_565
Cl1 Zr1 C8 80.5(4) 7_565 7_565
Cl1 Zr1 C8 104.5(4) . 7_565
C7 Zr1 C8 51.8(5) . 7_565
C7 Zr1 C8 31.0(5) 7_565 7_565
C6 Zr1 C8 53.5(6) . 7_565
C2 Zr1 C8 120.9(6) 7_565 7_565
C2 Zr1 C8 139.3(5) . 7_565
C1 Zr1 C8 118.8(6) . .
Cl1 Zr1 C8 104.5(4) 7_565 .
Cl1 Zr1 C8 80.5(4) . .
C7 Zr1 C8 31.0(5) . .
C7 Zr1 C8 51.8(5) 7_565 .
C6 Zr1 C8 53.5(6) . .
C2 Zr1 C8 139.3(5) 7_565 .
C2 Zr1 C8 120.9(6) . .
C8 Zr1 C8 31.1(8) 7_565 .
C1 Zr1 C3 54.3(6) . 7_565
Cl1 Zr1 C3 80.1(4) 7_565 7_565
Cl1 Zr1 C3 104.1(4) . 7_565
C7 Zr1 C3 142.6(5) . 7_565
C7 Zr1 C3 123.7(6) 7_565 7_565
C6 Zr1 C3 119.6(6) . 7_565
C2 Zr1 C3 34.3(5) 7_565 7_565
C2 Zr1 C3 54.5(5) . 7_565
C8 Zr1 C3 148.0(5) 7_565 7_565
C8 Zr1 C3 172.9(4) . 7_565
C1 Zr1 C3 54.3(6) . .
Cl1 Zr1 C3 104.1(4) 7_565 .
Cl1 Zr1 C3 80.1(4) . .
C7 Zr1 C3 123.7(6) . .
C7 Zr1 C3 142.6(5) 7_565 .
C6 Zr1 C3 119.6(6) . .
C2 Zr1 C3 54.5(6) 7_565 .
C2 Zr1 C3 34.3(5) . .
C8 Zr1 C3 172.9(4) 7_565 .
C8 Zr1 C3 148.0(5) . .
C3 Zr1 C3 31.2(8) 7_565 .
C10 Si1 C10 110.1(15) . 7_565
C10 Si1 C6 111.1(8) . .
C10 Si1 C6 111.1(8) 7_565 .
C10 Si1 C1 115.5(9) . .
C10 Si1 C1 115.5(9) 7_565 .
C6 Si1 C1 92.4(8) . .
C2 C1 C2 114(2) 7_565 .
C2 C1 Si1 122.1(12) 7_565 .
C2 C1 Si1 122.1(12) . .
C2 C1 Zr1 77.9(12) 7_565 .
C2 C1 Zr1 77.9(12) . .
Si1 C1 Zr1 100.5(10) . .
C1 C2 C3 105.8(19) . .
C1 C2 C4 136.2(19) . .
C3 C2 C4 118.0(17) . .
C1 C2 Zr1 70.0(12) . .
C3 C2 Zr1 76.1(8) . .
C4 C2 Zr1 118.0(14) . .
C3 C3 C5 124.4(12) 7_565 .
C3 C3 C2 107.1(11) 7_565 .
C5 C3 C2 128.0(19) . .
C3 C3 Zr1 74.4(4) 7_565 .
C5 C3 Zr1 127.4(11) . .
C2 C3 Zr1 69.6(7) . .
C7 C6 C7 101.0(19) 7_565 .
C7 C6 Si1 126.2(12) 7_565 .
C7 C6 Si1 126.2(12) . .
C7 C6 Zr1 71.1(10) 7_565 .
C7 C6 Zr1 71.1(10) . .
Si1 C6 Zr1 98.9(10) . .
C8 C7 C6 111.9(19) . .
C8 C7 Zr1 79.3(10) . .
C6 C7 Zr1 75.8(12) . .
C7 C8 C8 107.3(13) . 7_565
C7 C8 C9 144(3) . .
C8 C8 C9 108(2) 7_565 .
C7 C8 Zr1 69.8(10) . .
C8 C8 Zr1 74.4(4) 7_565 .
C9 C8 Zr1 123.3(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 C1 2.38(2) .
Zr1 Cl1 2.414(4) 7_565
Zr1 Cl1 2.414(4) .
Zr1 C7 2.421(16) .
Zr1 C7 2.421(16) 7_565
Zr1 C6 2.481(19) .
Zr1 C2 2.477(15) 7_565
Zr1 C2 2.477(15) .
Zr1 C8 2.535(16) 7_565
Zr1 C8 2.535(16) .
Zr1 C3 2.566(14) 7_565
Zr1 C3 2.566(14) .
Si1 C10 1.80(2) .
Si1 C10 1.80(2) 7_565
Si1 C6 1.86(2) .
Si1 C1 1.92(2) .
C1 C2 1.345(19) 7_565
C1 C2 1.345(19) .
C2 C3 1.49(2) .
C2 C4 1.50(3) .
C3 C3 1.38(4) 7_565
C3 C5 1.47(2) .
C6 C7 1.39(2) 7_565
C6 C7 1.394(19) .
C7 C8 1.33(2) .
C8 C8 1.36(4) 7_565
C8 C9 1.52(5) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139106482
