#------------------------------------------------------------------------------
#$Date: 2022-09-15 01:26:15 +0300 (Thu, 15 Sep 2022) $
#$Revision: 277847 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/02/4060230.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_4060230
loop_
_publ_author_name
'Józef Utko'
'Agnieszka Lizurek'
'Lucjan B. Jerzykiewicz'
'Piotr Sobota'
_publ_section_title
;
 Syntheses and Molecular Structure of [Mg2(OR)4(AlMe3)2] and
 [ZrCl3(OR)2(AlMe2)] (OR =1-methoxy-2-propoxide)
;
_journal_name_full               Organometallics
_journal_page_first              296
_journal_page_last               298
_journal_paper_doi               10.1021/om034263o
_journal_volume                  23
_journal_year                    2004
_chemical_formula_moiety         'C10 H24 Al Cl3 O4 Zr'
_chemical_formula_sum            'C10 H24 Al Cl3 O4 Zr'
_chemical_formula_weight         432.84
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_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            4
_cell_length_a                   18.340(4)
_cell_length_b                   10.932(2)
_cell_length_c                   9.062(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      8
_cell_volume                     1816.9(7)
_computing_cell_refinement       'Kuma KM4 software 1996'
_computing_data_collection       'Kuma KM4 software 1996'
_computing_data_reduction        'Kuma KM4 software 1996'
_computing_molecular_graphics    'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_publication_material  'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Kuma KM4 automatic diffractometer'
_diffrn_measurement_method       'profile data from omega-2theta scans'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3330
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.22
_diffrn_standards_interval_time  5.3
_diffrn_standards_number         100
_exptl_absorpt_coefficient_mu    1.099
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0376P)²+3.3724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                1427
_reflns_number_total             1696
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4060230
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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
Zr Zr 0.29774(2) 0.2500 0.39303(4) 0.01593(14) Uani 1 2 d S
Cl1 Cl 0.36365(6) 0.2500 0.62808(11) 0.0256(3) Uani 1 2 d S
Cl2 Cl 0.23929(6) 0.2500 0.15099(12) 0.0269(3) Uani 1 2 d S
Cl3 Cl 0.18406(7) 0.2500 0.53820(15) 0.0394(3) Uani 1 2 d S
Al Al 0.45381(7) 0.2500 0.24374(16) 0.0285(3) Uani 1 2 d S
O10 O 0.26821(13) 0.0460(2) 0.4007(2) 0.0311(5) Uani 1 1 d .
O11 O 0.38495(11) 0.14181(19) 0.3082(2) 0.0249(5) Uani 1 1 d .
C1 C 0.4639(3) 0.2500 0.0300(6) 0.0532(16) Uani 1 2 d S
H1A H 0.5151 0.2500 0.0028 0.080 Uiso 1 2 d SR
H1B H 0.4414 0.1783 -0.0092 0.080 Uiso 1 1 d R
C2 C 0.5408(3) 0.2500 0.3673(7) 0.0458(14) Uani 1 2 d S
H2A H 0.5616 0.1694 0.3690 0.069 Uiso 1 1 d R
H2B H 0.5276 0.2500 0.4658 0.069 Uiso 1 2 d SR
C11 C 0.4521(2) -0.0465(4) 0.2679(5) 0.0528(12) Uani 1 1 d .
H11A H 0.4474 -0.1334 0.2807 0.079 Uiso 1 1 calc R
H11B H 0.4936 -0.0178 0.3222 0.079 Uiso 1 1 calc R
H11C H 0.4584 -0.0283 0.1651 0.079 Uiso 1 1 calc R
C12 C 0.3865(3) 0.0140(4) 0.3224(10) 0.112(3) Uani 1 1 d .
H12 H 0.4037 0.0164 0.4247 0.134 Uiso 1 1 calc R
C13 C 0.3248(3) -0.0359(4) 0.3568(7) 0.089(2) Uani 1 1 d .
H13A H 0.3332 -0.0933 0.4366 0.106 Uiso 1 1 calc R
H13B H 0.3077 -0.0825 0.2725 0.106 Uiso 1 1 calc R
C14 C 0.1977(3) -0.0055(4) 0.3621(5) 0.0610(14) Uani 1 1 d .
H14A H 0.1965 -0.0228 0.2583 0.091 Uiso 1 1 calc R
H14B H 0.1600 0.0521 0.3861 0.091 Uiso 1 1 calc R
H14C H 0.1901 -0.0797 0.4165 0.091 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'
Al Al 0.0645 0.0514 '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'
O O 0.0106 0.0060 '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
O11 Zr O11 67.36(12) 8_565 .
O11 Zr O10 136.59(8) 8_565 .
O11 Zr O10 69.47(8) . .
O11 Zr O10 69.47(8) 8_565 8_565
O11 Zr O10 136.59(8) . 8_565
O10 Zr O10 152.48(13) . 8_565
O11 Zr Cl2 90.31(6) 8_565 .
O11 Zr Cl2 90.31(6) . .
O10 Zr Cl2 85.62(6) . .
O10 Zr Cl2 85.62(6) 8_565 .
O11 Zr Cl1 86.76(6) 8_565 .
O11 Zr Cl1 86.76(6) . .
O10 Zr Cl1 95.17(6) . .
O10 Zr Cl1 95.17(6) 8_565 .
Cl2 Zr Cl1 176.47(4) . .
O11 Zr Cl3 145.76(6) 8_565 .
O11 Zr Cl3 145.76(6) . .
O10 Zr Cl3 77.54(6) . .
O10 Zr Cl3 77.54(6) 8_565 .
Cl2 Zr Cl3 96.21(5) . .
Cl1 Zr Cl3 87.32(5) . .
O11 Zr Al 33.68(6) 8_565 .
O11 Zr Al 33.68(6) . .
O10 Zr Al 103.08(6) . .
O10 Zr Al 103.08(6) 8_565 .
Cl2 Zr Al 90.75(4) . .
Cl1 Zr Al 85.72(4) . .
Cl3 Zr Al 173.05(4) . .
O11 Al O11 80.74(14) . 8_565
O11 Al C1 112.57(16) . .
O11 Al C1 112.57(16) 8_565 .
O11 Al C2 112.47(16) . .
O11 Al C2 112.47(16) 8_565 .
C1 Al C2 119.6(3) . .
O11 Al Zr 40.37(7) . .
O11 Al Zr 40.37(7) 8_565 .
C1 Al Zr 120.74(19) . .
C2 Al Zr 119.63(19) . .
C13 O10 C14 109.7(4) . .
C13 O10 Zr 115.4(2) . .
C14 O10 Zr 125.4(2) . .
C12 O11 Al 131.3(3) . .
C12 O11 Zr 122.3(3) . .
Al O11 Zr 105.95(10) . .
C13 C12 O11 115.1(4) . .
C13 C12 C11 127.7(4) . .
O11 C12 C11 115.9(4) . .
C12 C13 O10 116.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr O11 2.133(2) 8_565
Zr O11 2.133(2) .
Zr O10 2.296(2) .
Zr O10 2.296(2) 8_565
Zr Cl2 2.4413(12) .
Zr Cl1 2.4491(12) .
Zr Cl3 2.4653(13) .
Zr Al 3.1659(15) .
Al O11 1.826(2) .
Al O11 1.826(2) 8_565
Al C1 1.946(6) .
Al C2 1.948(5) .
O10 C13 1.428(5) .
O10 C14 1.453(4) .
O11 C12 1.404(5) .
C11 C12 1.459(6) .
C12 C13 1.293(7) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C13 H13B Cl3 0.9700 2.8100 3.7201 157.00 2_554 yes
C13 H13B Cl3 0.9700 2.8100 3.7201 157.00 7_544 yes
C14 H14B Cl3 0.9600 2.6000 3.2261 123.00 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O11 Zr Al O11 -178.9(2) 8_565 .
O10 Zr Al O11 -3.75(13) . .
O10 Zr Al O11 -175.11(12) 8_565 .
Cl2 Zr Al O11 -89.43(11) . .
Cl1 Zr Al O11 90.57(11) . .
Cl3 Zr Al O11 90.57(11) . .
O11 Zr Al O11 178.9(2) . 8_565
O10 Zr Al O11 175.11(12) . 8_565
O10 Zr Al O11 3.75(13) 8_565 8_565
Cl2 Zr Al O11 89.43(11) . 8_565
Cl1 Zr Al O11 -90.57(11) . 8_565
Cl3 Zr Al O11 -90.57(11) . 8_565
O11 Zr Al C1 -89.43(11) 8_565 .
O11 Zr Al C1 89.43(11) . .
O10 Zr Al C1 85.68(6) . .
O10 Zr Al C1 -85.68(6) 8_565 .
Cl2 Zr Al C1 0.0 . .
Cl1 Zr Al C1 180.0 . .
Cl3 Zr Al C1 180.0 . .
O11 Zr Al C2 90.57(11) 8_565 .
O11 Zr Al C2 -90.57(11) . .
O10 Zr Al C2 -94.32(6) . .
O10 Zr Al C2 94.32(6) 8_565 .
Cl2 Zr Al C2 180.0 . .
Cl1 Zr Al C2 0.0 . .
Cl3 Zr Al C2 0.0 . .
O11 Zr O10 C13 10.7(4) 8_565 .
O11 Zr O10 C13 4.5(4) . .
O10 Zr O10 C13 168.2(3) 8_565 .
Cl2 Zr O10 C13 96.5(4) . .
Cl1 Zr O10 C13 -80.1(4) . .
Cl3 Zr O10 C13 -166.2(4) . .
Al Zr O10 C13 6.7(4) . .
O11 Zr O10 C14 -132.0(3) 8_565 .
O11 Zr O10 C14 -138.2(3) . .
O10 Zr O10 C14 25.6(4) 8_565 .
Cl2 Zr O10 C14 -46.2(3) . .
Cl1 Zr O10 C14 137.2(3) . .
Cl3 Zr O10 C14 51.1(3) . .
Al Zr O10 C14 -136.0(3) . .
O11 Al O11 C12 -173.0(5) 8_565 .
C1 Al O11 C12 76.3(6) . .
C2 Al O11 C12 -62.4(6) . .
Zr Al O11 C12 -172.3(6) . .
O11 Al O11 Zr -0.75(14) 8_565 .
C1 Al O11 Zr -111.45(16) . .
C2 Al O11 Zr 109.84(16) . .
O11 Zr O11 C12 173.8(5) 8_565 .
O10 Zr O11 C12 -10.8(5) . .
O10 Zr O11 C12 -179.9(5) 8_565 .
Cl2 Zr O11 C12 -96.0(5) . .
Cl1 Zr O11 C12 86.0(5) . .
Cl3 Zr O11 C12 5.6(5) . .
Al Zr O11 C12 173.1(5) . .
O11 Zr O11 Al 0.68(13) 8_565 .
O10 Zr O11 Al 176.09(13) . .
O10 Zr O11 Al 6.95(17) 8_565 .
Cl2 Zr O11 Al 90.89(10) . .
Cl1 Zr O11 Al -87.15(10) . .
Cl3 Zr O11 Al -167.58(8) . .
Al O11 C12 C13 -172.7(5) . .
Zr O11 C12 C13 16.1(10) . .
Al O11 C12 C11 -4.7(10) . .
Zr O11 C12 C11 -175.9(4) . .
O11 C12 C13 O10 -10.7(11) . .
C11 C12 C13 O10 -177.1(7) . .
C14 O10 C13 C12 150.4(7) . .
Zr O10 C13 C12 2.0(9) . .
