#------------------------------------------------------------------------------
#$Date: 2017-02-13 17:11:48 +0200 (Mon, 13 Feb 2017) $
#$Revision: 192024 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/41/2004124.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_2004124
loop_
_publ_author_name
'Jardin, M.'
'Gao, Y.'
'Guéry, J.'
'Jacoboni, C.'
_publ_section_title
Chlorotris(2,2,6,6-tetramethyl-3,5-heptanedionato-O,O')zirconium(IV)
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2230
_journal_page_last               2232
_journal_paper_doi               10.1107/S0108270195006494
_journal_volume                  51
_journal_year                    1995
_chemical_formula_analytical     'C33.9 H58 O6 Cl1.1 Zr1'
_chemical_formula_moiety         'C33 H57 Cl1 O6 Zr1'
_chemical_formula_structural     '[Zr (C11 H19 O2)3 Cl]'
_chemical_formula_sum            'C33 H57 Cl O6 Zr'
_chemical_formula_weight         676.48
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 117.706(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6883(6)
_cell_length_b                   18.270(2)
_cell_length_c                   10.9819(7)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293
_cell_measurement_theta_max      32
_cell_measurement_theta_min      31
_cell_volume                     1898.6(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'SCHAKAL92 (Keller, 1992)'
_computing_structure_refinement  SHELX76
_computing_structure_solution    'SHELX76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Stoe Siemens AED2'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Fine focus Siemens Mo X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9716
_diffrn_reflns_theta_max         35
_diffrn_reflns_theta_min         0.5
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   'SHELX76 Gaussian (Sheldrick, 1976)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       needle
_exptl_crystal_F_000             713.99
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.212
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.041
_refine_ls_shift/esd_max         0.520
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.041
_reflns_number_observed          4125
_reflns_number_total             7420
_reflns_observed_criterion       refl_observed_if_I_>_6.0_\s(I)
_cod_data_source_file            du1125.cif
_cod_data_source_block           ZrDPM3Cl
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '?' to '1'
 for all fully occupied atom sites. The occupancies for atoms 'H12a',
 'H181', 'H182' and 'H183' were determined from the occupancy of atom
 'C(18)' that they are bonded to.

 Antanas Vaitkus,
 2017-02-13
;
_cod_original_cell_volume        1898.5(2)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C33 H57 Cl1 O6 Zr1'
_cod_database_code               2004124
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,1/2+y,-z
-x,-y,-z
x,1/2-y,z
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_refinement_flags
_atom_site_type_symbol
Zr 1 0.15192(4) 0.25 0.12551(4) 0.041(3) Uani ? Zr
Cl 1 0.2498(1) 0.25 0.3810(1) 0.07(1) Uani ? Cl
O(1) 1 0.9310(3) 0.25 0.9876(3) 0.051(3) Uani ? O
O(2) 1 0.1413(3) 0.25 0.9286(3) 0.056(3) Uani ? O
O(3) 1 0.3205(2) 0.1768(1) 0.1563(2) 0.056(1) Uani ? O
O(4) 1 0.0753(2) 0.1459(1) 0.1480(2) 0.053(1) Uani ? O
C(1) 1 0.8519(4) 0.25 0.8598(4) 0.046(3) Uani ? C
C(2) 1 0.0473(4) 0.25 0.8022(4) 0.047(4) Uani ? C
C(3) 1 0.1049(5) 0.25 0.6988(4) 0.056(4) Uani ? C
C(4) 1 0.3563(3) 0.1124(2) 0.2053(3) 0.052(3) Uani ? C
C(5) 1 0.9048(4) 0.25 0.7653(5) 0.057(4) Uani ? C
C(6) 1 0.6925(4) 0.25 0.8126(5) 0.053(4) Uani ? C
C(7) 1 0.1339(3) 0.0859(2) 0.2074(3) 0.053(3) Uani ? C
C(8) 1 0.2702(3) 0.0675(2) 0.2359(4) 0.061(3) Uani ? C
C(9) 1 0.5039(3) 0.0891(2) 0.2305(4) 0.062(3) Uani ? C
C(10) 1 0.0417(4) 0.0365(2) 0.2448(4) 0.068(4) Uani ? C
C(11) 1 0.2000(4) 0.1824(2) 0.7259(4) 0.082(4) Uani ? C
C(12) 1 0.9901(7) 0.25 0.5502(6) 0.092(6) Uani ? C
C(13) 1 0.5165(6) 0.1066(4) 0.1026(6) 0.155(8) Uani ? C
C(14) 1 0.5335(5) 0.0082(3) 0.2608(7) 0.128(6) Uani ? C
C(15) 1 0.8954(5) 0.0315(4) 0.1256(6) 0.149(7) Uani ? C
C(16) 1 0.6080(5) 0.1342(3) 0.3453(7) 0.167(8) Uani ? C
C(17) 1 0.020(1) 0.0754(5) 0.3516(7) 0.23(1) Uani ? C
C(18) 0.5 0.6643(7) 0.2797(8) 0.9290(8) 0.13(1) Uani ? C
C(19) 1 0.6244(6) 0.1895(4) 0.721(1) 0.27(1) Uani ? C
C(20) 1 0.1062(7) 0.9636(3) 0.297(1) 0.25(1) Uani ? C
H(5) 1 0.8420(5) 0.25 0.674(5) 0.06(1) Uiso ? H
H(8) 1 0.306(4) 0.025(2) 0.274(4) 0.08(1) Uiso ? H
H(111) 1 0.278(4) 0.1858(2) 0.8330(4) 0.174(5) Uiso G H
H(112) 1 0.2524(4) 0.1846(2) 0.6622(4) 0.174(4) Uiso G H
H(113) 1 0.1424(4) 0.1316(2) 0.7077(4) 0.174(4) Uiso G H
H(121) 1 0.924(4) 0.206(2) 0.527(4) 0.11(1) Uiso ? H
H(122) 1 0.032(5) 0.25 0.489(5) 0.08(1) Uiso ? H
H(131) 1 0.4431(6) 0.0805(4) 0.0076(6) 0.174(4) Uiso G H
H(132) 1 0.6235(6) 0.0958(4) 0.1214(6) 0.174(4) Uiso G H
H(133) 1 0.4980(6) 0.1649(4) 0.0946(6) 0.174(4) Uiso G H
H(141) 1 0.5315(5) 0.0020(3) 0.3577(7) 0.174(4) Uiso G H
H(142) 1 0.6388(5) 0.9969(3) 0.2751(7) 0.174(4) Uiso G H
H(143) 1 0.4596(5) 0.9703(3) 0.1866(7) 0.174(4) Uiso G H
H(151) 1 0.9562(5) 0.9917(4) 0.1026(6) 0.174(4) Uiso G H
H(152) 1 0.8367(5) 0.0655(4) 0.0363(6) 0.174(4) Uiso G H
H(153) 1 0.8227(5) 0.0036(4) 0.1528(6) 0.174(4) Uiso G H
H(161) 1 0.5876(5) 0.0953(3) 0.4079(7) 0.174(4) Uiso G H
H(162) 1 0.5970(5) 0.1891(3) 0.3755(7) 0.174(4) Uiso G H
H(163) 1 0.7142(5) 0.1266(3) 0.3593(7) 0.174(4) Uiso G H
H(171) 1 0.120(1) 0.0472(5) 0.4040(7) 0.174(4) Uiso G H
H(172) 1 0.941(1) 0.0469(5) 0.3694(7) 0.174(4) Uiso G H
H(173) 1 0.031(1) 0.1306(5) 0.3905(7) 0.174(4) Uiso G H
H(181) 0.5 0.5527(7) 0.2765(8) 0.8988(8) 0.174(4) Uiso G H
H(182) 0.5 0.6900(7) 0.3342(8) 0.9095(8) 0.174(4) Uiso G H
H(183) 0.5 0.7245(7) 0.2675(8) 0.0374(8) 0.174(4) Uiso G H
H(191) 1 0.6595(6) 0.1734(4) 0.826(1) 0.174(4) Uiso G H
H(192) 1 0.6553(6) 0.1483(4) 0.669(1) 0.174(4) Uiso G H
H(193) 1 0.5106(6) 0.1950(4) 0.669(1) 0.174(4) Uiso G H
H(201) 1 0.0482(7) 0.9509(3) 0.188(1) 0.174(4) Uiso G H
H(202) 1 0.0497(7) 0.9425(3) 0.349(1) 0.174(4) Uiso G H
H(203) 1 0.2097(7) 0.9389(3) 0.339(1) 0.174(4) Uiso G H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
Zr Zr4+ International_Tables_Vol_IV_Table_2.2B -2.965 0.560
Cl Cl1- International_Tables_Vol_IV_Table_2.2B 0.132 0.159
C C International_Tables_Vol_IV_Table_2.2B 0.002 0.002
H H International_Tables_Vol_IV_Table_2.2B 0.0 0.0
O O International_Tables_Vol_IV_Table_2.2B 0.008 0.006
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 0 1
-3 7 1
-3 -7 1
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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl Zr O(2) . . 1_554 161.0(2) yes
Cl Zr O(4) . . . 81.50(10) yes
Cl Zr O(1) . . 1_454 123.00(10) yes
Cl Zr O(3) . . . 86.60(10) yes
O(1) Zr O(2) 1_454 . 1_554 76.0(2) yes
O(1) Zr O(4) 1_454 . . 74.0(2) yes
O(3) Zr O(2) . . 1_554 78.6(2) yes
O(3) Zr O(4) . . 4_555 151.7(2) yes
O(3) Zr O(4) . . . 76.3(2) yes
O(3) Zr O(1) . . 1_454 133.2(2) yes
O(3) Zr O(3) . . 4_555 77.4(2) yes
O(4) Zr O(2) . . 1_554 106.1(2) yes
O(4) Zr O(4) . . 4_555 126.5(2) yes
C(1) O(1) Zr . 1_454 . 137.7(3) yes
C(2) O(2) Zr . 1_554 . 138.7(3) yes
C(4) O(3) Zr . . . 135.0(2) yes
C(7) O(4) Zr . . . 134.4(2) yes
O(1) C(1) C(5) . . . 122.5(4) yes
O(1) C(1) C(6) . . . 116.2(4) yes
C(5) C(1) C(6) . . . 121.4(4) yes
O(2) C(2) C(5) 1_554 1_554 1_454 121.4(5) yes
O(2) C(2) C(3) . . . 115.0(4) yes
C(5) C(2) C(3) 1_454 1_554 1_554 123.6(3) yes
C(11) C(3) C(11) . . 4_555 106.8(4) yes
C(12) C(3) C(11) 1_454 1_554 1_554 109.8(3) yes
O(3) C(4) C(8) . . . 123.1(3) yes
O(3) C(4) C(9) . . . 114.5(3) yes
C(8) C(4) C(9) . . . 122.4(3) yes
C(2) C(5) C(1) 1_554 1_454 1_454 123.7(4) yes
C(19) C(6) C(19) . . 4_555 99.9(6) yes
C(19) C(6) C(18) . . . 128.1(5) yes
O(4) C(7) C(8) . . . 122.6(3) yes
O(4) C(7) C(10) . . . 114.8(3) yes
C(8) C(7) C(10) . . . 122.6(3) yes
C(7) C(8) C(4) . . . 123.3(3) yes
C(16) C(9) C(13) . . . 108.5(4) yes
C(16) C(9) C(14) . . . 111.0(3) yes
C(13) C(9) C(14) . . . 108.1(5) yes
C(17) C(10) C(20) . . 1_545 110.1(6) yes
C(17) C(10) C(15) . . 1_455 103.5(5) yes
C(20) C(10) C(15) 1_545 . 1_455 112.8(4) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr Cl . . 2.4950(10) yes
Zr O(1) . 1_454 2.130(2) yes
Zr O(2) . 1_554 2.110(3) yes
Zr O(3) . . 2.140(2) yes
Zr O(4) . . 2.129(2) yes
O(1) O(2) 1_454 1_554 2.611(3) yes
O(1) O(4) 1_454 . 2.562(3) yes
O(1) C(1) . . 1.258(4) yes
O(2) C(2) . . 1.281(4) yes
O(3) Cl . . 3.189(2) yes
O(3) O(2) . 1_554 2.692(3) yes
O(3) O(3) . 4_555 2.676(3) yes
O(3) O(4) . . 2.638(3) yes
O(3) C(4) . . 1.275(4) yes
O(4) Cl . . 3.032(2) yes
O(4) C(7) . . 1.281(4) yes
C(2) C(3) . . 1.523(8) yes
C(2) C(5) 1_554 1_454 1.382(6) yes
C(3) C(11) . . 1.538(5) yes
C(3) C(12) 1_554 1_454 1.518(6) yes
C(4) C(8) . . 1.386(6) yes
C(4) C(9) . . 1.531(5) yes
C(5) C(1) . . 1.393(8) yes
C(6) C(1) . . 1.533(6) yes
C(6) C(19) . . 1.445(8) yes
C(6) C(18) . . 1.540(10) yes
C(7) C(8) . . 1.383(5) yes
C(7) C(10) . . 1.527(6) yes
C(9) C(13) . . 1.507(9) yes
C(9) C(14) . . 1.516(6) yes
C(9) C(16) . . 1.484(6) yes
C(10) C(15) . 1_455 1.505(5) yes
C(10) C(17) . . 1.480(10) yes
C(10) C(20) . 1_545 1.485(7) yes
