#------------------------------------------------------------------------------
#$Date: 2016-02-04 08:09:49 +0200 (Thu, 04 Feb 2016) $
#$Revision: 175770 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/37/4513730.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_4513730
loop_
_publ_author_name
'Crochet, Aurélien'
'Brog, Jean-Pierre'
'Fromm, Katharina M.'
_publ_section_title
;
 Mixed Metal Multinuclear Cr(III) Cage Compounds and Coordination Polymers
 Based on Unsubstituted Phenolate: Design, Synthesis, Mechanism, and
 Properties
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              189
_journal_paper_doi               10.1021/acs.cgd.5b01084
_journal_volume                  16
_journal_year                    2016
_chemical_formula_moiety         'Cr Cl2 (O C4 H8)2'
_chemical_formula_sum            'C8 H16 Cl2 Cr O2'
_chemical_formula_weight         267.11
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.918(4)
_cell_angle_beta                 79.841(4)
_cell_angle_gamma                87.105(4)
_cell_formula_units_Z            1
_cell_length_a                   3.9645(2)
_cell_length_b                   7.2398(4)
_cell_length_c                   9.2813(5)
_cell_measurement_reflns_used    16246
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.12
_cell_measurement_theta_min      2.23
_cell_volume                     261.61(2)
_computing_cell_refinement       X-Area
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            924
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             138
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.344
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0402
_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)+(0.0781P)²+1.5609P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                768
_reflns_number_total             924
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            1.cif
_cod_data_source_block           '[CrCl2(THF)2]n'
_cod_depositor_comments
'Adding full bibliography for 4513725--4513731.cif.'
_cod_database_code               4513730
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cr1 Cr 1.0000 0.0000 1.0000 0.0105(3) Uani 1 2 d S . P
Cl1 Cl 1.3879(3) -0.19611(14) 1.11958(11) 0.0127(3) Uani 1 1 d . . .
O1 O 0.9084(9) 0.1644(4) 1.1796(3) 0.0155(7) Uani 1 1 d . . .
C4 C 0.9287(12) 0.3652(6) 1.1729(5) 0.0124(9) Uani 1 1 d . . .
H4A H 0.7982 0.4224 1.0992 0.015 Uiso 1 1 calc R U .
H4B H 1.1702 0.4012 1.1466 0.015 Uiso 1 1 calc R U .
C1 C 0.7760(13) 0.0964(6) 1.3277(5) 0.0135(10) Uani 1 1 d . . .
H1A H 0.9055 -0.0174 1.3537 0.016 Uiso 1 1 calc R U .
H1B H 0.5304 0.0691 1.3384 0.016 Uiso 1 1 calc R U .
C2 C 0.8247(12) 0.2526(7) 1.4233(5) 0.0136(10) Uani 1 1 d . . .
H2A H 1.0576 0.2453 1.4485 0.016 Uiso 1 1 calc R U .
H2B H 0.6528 0.2511 1.5147 0.016 Uiso 1 1 calc R U .
C3 C 0.7725(12) 0.4257(6) 1.3256(5) 0.0125(10) Uani 1 1 d . . .
H3A H 0.5259 0.4608 1.3322 0.015 Uiso 1 1 calc R U .
H3B H 0.8928 0.5315 1.3530 0.015 Uiso 1 1 calc R U .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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
O1 Cr1 O1 180.0 2_757 .
O1 Cr1 Cl1 90.52(10) 2_757 .
O1 Cr1 Cl1 89.48(10) . .
O1 Cr1 Cl1 89.48(10) 2_757 2_757
O1 Cr1 Cl1 90.52(10) . 2_757
Cl1 Cr1 Cl1 180.0 . 2_757
C1 O1 C4 110.8(3) . .
C1 O1 Cr1 123.9(3) . .
C4 O1 Cr1 125.0(3) . .
O1 C4 C3 105.4(4) . .
O1 C4 H4A 110.7 . .
C3 C4 H4A 110.7 . .
O1 C4 H4B 110.7 . .
C3 C4 H4B 110.7 . .
H4A C4 H4B 108.8 . .
O1 C1 C2 104.5(4) . .
O1 C1 H1A 110.8 . .
C2 C1 H1A 110.8 . .
O1 C1 H1B 110.8 . .
C2 C1 H1B 110.8 . .
H1A C1 H1B 108.9 . .
C1 C2 C3 102.8(4) . .
C1 C2 H2A 111.2 . .
C3 C2 H2A 111.2 . .
C1 C2 H2B 111.2 . .
C3 C2 H2B 111.2 . .
H2A C2 H2B 109.1 . .
C4 C3 C2 103.1(4) . .
C4 C3 H3A 111.1 . .
C2 C3 H3A 111.1 . .
C4 C3 H3B 111.1 . .
C2 C3 H3B 111.1 . .
H3A C3 H3B 109.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O1 2.070(3) 2_757
Cr1 O1 2.070(3) .
Cr1 Cl1 2.4133(10) .
Cr1 Cl1 2.4133(10) 2_757
O1 C1 1.451(5) .
O1 C4 1.457(5) .
C4 C3 1.522(6) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C1 C2 1.514(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.533(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
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
C1 O1 C4 C3 -4.4(5)
Cr1 O1 C4 C3 168.9(3)
C4 O1 C1 C2 -18.4(5)
Cr1 O1 C1 C2 168.2(3)
O1 C1 C2 C3 33.3(5)
O1 C4 C3 C2 25.0(5)
C1 C2 C3 C4 -35.7(5)
