#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:20:16 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180008 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/02/7030275.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_7030275
loop_
_publ_author_name
'Benjamin, Sophie L.'
'Levason, William'
'Pugh, David'
'Reid, Gillian'
'Zhang, Wenjian'
_publ_section_title
;
 Preparation and structures of coordination complexes of the very hard
 Lewis acids ZrF4 and HfF4.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12548
_journal_page_last               12557
_journal_paper_doi               10.1039/c2dt31501g
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C36 H30 As2 F4 O2 Zr, 2(C H2 Cl2)'
_chemical_formula_structural     '((C18 H15 As O)2 (F4 Zr)) (C H2 Cl2)2'
_chemical_formula_sum            'C38 H34 As2 Cl4 F4 O2 Zr'
_chemical_formula_weight         981.51
_chemical_name_systematic
;
trans-tetrafluoro-bis(triphenylarsine oxide)-zirconium(IV)
dichloromethane solvate
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-06
_audit_creation_method           'SHELXL-97 hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.348(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.898(3)
_cell_length_b                   14.688(4)
_cell_length_c                   14.840(5)
_cell_measurement_reflns_used    7000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1933.9(11)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9087
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.312
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998). REQAB. Private communication to the
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colourless
_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          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0118P)²+15.6494P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                3571
_reflns_number_total             4383
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c2dt31501g.txt
_cod_data_source_block           12slbrwl6x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1933.8(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7030275
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.5000 0.5000 0.0000 0.01212(15) Uani 1 2 d S
As1 As 0.40282(6) 0.45349(3) 0.22678(3) 0.01498(13) Uani 1 1 d .
F1 F 0.3483(4) 0.5957(2) 0.0221(2) 0.0246(7) Uani 1 1 d .
F2 F 0.3382(4) 0.4169(2) -0.0514(2) 0.0236(7) Uani 1 1 d .
O1 O 0.4767(4) 0.4428(2) 0.1274(2) 0.0185(8) Uani 1 1 d .
C1 C 0.4519(6) 0.3460(3) 0.2947(3) 0.0181(10) Uani 1 1 d .
C2 C 0.5980(7) 0.3141(4) 0.2989(4) 0.0313(14) Uani 1 1 d .
H2 H 0.6726 0.3457 0.2686 0.038 Uiso 1 1 calc R
C3 C 0.6350(7) 0.2360(4) 0.3472(5) 0.0351(16) Uani 1 1 d .
H3 H 0.7346 0.2125 0.3486 0.042 Uiso 1 1 calc R
C4 C 0.5269(7) 0.1918(4) 0.3938(4) 0.0271(13) Uani 1 1 d .
H4 H 0.5541 0.1402 0.4300 0.033 Uiso 1 1 calc R
C5 C 0.3808(7) 0.2226(4) 0.3878(4) 0.0251(12) Uani 1 1 d .
H5 H 0.3057 0.1901 0.4167 0.030 Uiso 1 1 calc R
C6 C 0.3425(6) 0.3015(4) 0.3392(4) 0.0236(12) Uani 1 1 d .
H6 H 0.2424 0.3244 0.3367 0.028 Uiso 1 1 calc R
C7 C 0.4919(6) 0.5569(3) 0.2893(4) 0.0182(10) Uani 1 1 d .
C8 C 0.5637(7) 0.5469(4) 0.3759(4) 0.0259(12) Uani 1 1 d .
H8 H 0.5692 0.4892 0.4048 0.031 Uiso 1 1 calc R
C9 C 0.6258(8) 0.6224(5) 0.4177(5) 0.0385(16) Uani 1 1 d .
H9 H 0.6746 0.6166 0.4767 0.046 Uiso 1 1 calc R
C10 C 0.6196(7) 0.7063(4) 0.3770(5) 0.0347(15) Uani 1 1 d .
H10 H 0.6635 0.7578 0.4073 0.042 Uiso 1 1 calc R
C11 C 0.5482(7) 0.7152(4) 0.2908(4) 0.0275(13) Uani 1 1 d .
H11 H 0.5425 0.7731 0.2623 0.033 Uiso 1 1 calc R
C12 C 0.4856(6) 0.6400(4) 0.2463(4) 0.0226(11) Uani 1 1 d .
H12 H 0.4388 0.6456 0.1868 0.027 Uiso 1 1 calc R
C13 C 0.1898(6) 0.4681(3) 0.2112(4) 0.0173(10) Uani 1 1 d .
C14 C 0.1148(6) 0.5013(4) 0.2834(4) 0.0241(12) Uani 1 1 d .
H14 H 0.1697 0.5199 0.3377 0.029 Uiso 1 1 calc R
C15 C -0.0421(7) 0.5070(4) 0.2747(4) 0.0308(14) Uani 1 1 d .
H15 H -0.0955 0.5272 0.3240 0.037 Uiso 1 1 calc R
C16 C -0.1188(6) 0.4831(4) 0.1947(4) 0.0269(13) Uani 1 1 d .
H16 H -0.2256 0.4882 0.1888 0.032 Uiso 1 1 calc R
C17 C -0.0442(6) 0.4516(4) 0.1219(4) 0.0227(11) Uani 1 1 d .
H17 H -0.0996 0.4359 0.0668 0.027 Uiso 1 1 calc R
C18 C 0.1119(6) 0.4430(3) 0.1298(4) 0.0193(11) Uani 1 1 d .
H18 H 0.1643 0.4206 0.0810 0.023 Uiso 1 1 calc R
Cl1 Cl 0.5239(2) 0.86462(14) 1.02974(16) 0.0569(6) Uani 1 1 d .
Cl2 Cl 0.7229(2) 0.78527(12) 0.90399(13) 0.0460(5) Uani 1 1 d .
C19A C 0.5563(9) 0.7731(5) 0.9573(6) 0.036(2) Uani 0.850(14) 1 d P
H19A H 0.5607 0.7158 0.9926 0.043 Uiso 0.850(14) 1 calc PR
H19B H 0.4707 0.7683 0.9108 0.043 Uiso 0.850(14) 1 calc PR
C19B C 0.696(4) 0.846(2) 0.998(2) 0.016(8) Uiso 0.150(14) 1 d P
H19C H 0.7538 0.8155 1.0486 0.020 Uiso 0.150(14) 1 calc PR
H19D H 0.7431 0.9062 0.9902 0.020 Uiso 0.150(14) 1 calc PR
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
Cl Cl 0.1484 0.1585 '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
F1 Zr1 F1 180.00(18) 3_665 .
F1 Zr1 F2 89.08(13) 3_665 .
F1 Zr1 F2 90.92(14) . .
F1 Zr1 F2 90.92(13) 3_665 3_665
F1 Zr1 F2 89.08(13) . 3_665
F2 Zr1 F2 180.0(2) . 3_665
F1 Zr1 O1 88.88(13) 3_665 .
F1 Zr1 O1 91.12(13) . .
F2 Zr1 O1 88.97(14) . .
F2 Zr1 O1 91.03(14) 3_665 .
F1 Zr1 O1 91.12(13) 3_665 3_665
F1 Zr1 O1 88.88(13) . 3_665
F2 Zr1 O1 91.03(14) . 3_665
F2 Zr1 O1 88.97(14) 3_665 3_665
O1 Zr1 O1 180.00(18) . 3_665
O1 As1 C13 111.0(2) . .
O1 As1 C1 107.4(2) . .
C13 As1 C1 110.1(2) . .
O1 As1 C7 109.0(2) . .
C13 As1 C7 109.9(2) . .
C1 As1 C7 109.3(2) . .
As1 O1 Zr1 146.5(2) . .
C2 C1 C6 121.0(5) . .
C2 C1 As1 118.8(4) . .
C6 C1 As1 120.2(4) . .
C3 C2 C1 119.5(5) . .
C3 C2 H2 120.2 . .
C1 C2 H2 120.2 . .
C2 C3 C4 120.0(6) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C5 C4 C3 120.2(5) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 120.1(5) . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C1 C6 C5 119.1(5) . .
C1 C6 H6 120.4 . .
C5 C6 H6 120.4 . .
C12 C7 C8 121.3(5) . .
C12 C7 As1 118.4(4) . .
C8 C7 As1 120.3(4) . .
C9 C8 C7 118.2(6) . .
C9 C8 H8 120.9 . .
C7 C8 H8 120.9 . .
C8 C9 C10 121.8(6) . .
C8 C9 H9 119.1 . .
C10 C9 H9 119.1 . .
C9 C10 C11 119.4(6) . .
C9 C10 H10 120.3 . .
C11 C10 H10 120.3 . .
C12 C11 C10 120.3(6) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C7 C12 C11 119.0(5) . .
C7 C12 H12 120.5 . .
C11 C12 H12 120.5 . .
C14 C13 C18 121.5(5) . .
C14 C13 As1 118.5(4) . .
C18 C13 As1 119.9(4) . .
C13 C14 C15 119.0(5) . .
C13 C14 H14 120.5 . .
C15 C14 H14 120.5 . .
C16 C15 C14 119.6(5) . .
C16 C15 H15 120.2 . .
C14 C15 H15 120.2 . .
C15 C16 C17 121.5(5) . .
C15 C16 H16 119.2 . .
C17 C16 H16 119.2 . .
C16 C17 C18 119.8(5) . .
C16 C17 H17 120.1 . .
C18 C17 H17 120.1 . .
C17 C18 C13 118.4(5) . .
C17 C18 H18 120.8 . .
C13 C18 H18 120.8 . .
C19B Cl1 C19A 60.0(12) . .
C19B Cl2 C19A 60.0(12) . .
Cl2 C19A Cl1 112.5(4) . .
Cl2 C19A H19A 109.1 . .
Cl1 C19A H19A 109.1 . .
Cl2 C19A H19B 109.1 . .
Cl1 C19A H19B 109.1 . .
H19A C19A H19B 107.8 . .
Cl1 C19B Cl2 121(2) . .
Cl1 C19B H19C 107.0 . .
Cl2 C19B H19C 107.0 . .
Cl1 C19B H19D 107.0 . .
Cl2 C19B H19D 107.0 . .
H19C C19B H19D 106.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 F1 1.993(3) 3_665
Zr1 F1 1.993(3) .
Zr1 F2 1.994(3) .
Zr1 F2 1.994(3) 3_665
Zr1 O1 2.093(3) .
Zr1 O1 2.093(3) 3_665
As1 O1 1.668(3) .
As1 C13 1.905(5) .
As1 C1 1.906(5) .
As1 C7 1.920(5) .
C1 C2 1.378(8) .
C1 C6 1.381(7) .
C2 C3 1.380(8) .
C2 H2 0.9500 .
C3 C4 1.388(8) .
C3 H3 0.9500 .
C4 C5 1.373(9) .
C4 H4 0.9500 .
C5 C6 1.393(8) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C12 1.377(7) .
C7 C8 1.398(8) .
C8 C9 1.367(9) .
C8 H8 0.9500 .
C9 C10 1.372(10) .
C9 H9 0.9500 .
C10 C11 1.391(9) .
C10 H10 0.9500 .
C11 C12 1.382(8) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.392(7) .
C13 C18 1.396(7) .
C14 C15 1.395(8) .
C14 H14 0.9500 .
C15 C16 1.370(9) .
C15 H15 0.9500 .
C16 C17 1.390(8) .
C16 H16 0.9500 .
C17 C18 1.390(7) .
C17 H17 0.9500 .
C18 H18 0.9500 .
Cl1 C19B 1.66(3) .
Cl1 C19A 1.759(7) .
Cl2 C19B 1.68(3) .
Cl2 C19A 1.741(7) .
C19A H19A 0.9900 .
C19A H19B 0.9900 .
C19B H19C 0.9900 .
C19B H19D 0.9900 .
