#------------------------------------------------------------------------------
#$Date: 2020-11-05 10:56:28 +0200 (Thu, 05 Nov 2020) $
#$Revision: 258736 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/81/4318157.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_4318157
loop_
_publ_author_name
'Philip G. Jessop'
'Marilyn M. Olmstead'
'Christopher D. Ablan'
'Megan Grabenauer'
'Daniel Sheppard'
'Charles A. Eckert'
'Charles L. Liotta'
_publ_section_title
;
 Carbon Dioxide as a Solubility "Switch" for the Reversible Dissolution of
 Highly Fluorinated Complexes and Reagents in Organic Solvents:
 Application to Crystallization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3463
_journal_page_last               3468
_journal_paper_doi               10.1021/ic020057h
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C15 H3 Cr F18 O6'
_chemical_formula_weight         673.17
_chemical_name_common            Cr(hfacac)3
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.067(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7318(12)
_cell_length_b                   12.9417(17)
_cell_length_c                   19.074(3)
_cell_measurement_reflns_used    654
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.5
_cell_volume                     2154.0(5)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29586
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0451P)²+1.7741P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                5326
_reflns_number_total             6235
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic020057h_3.cif
_cod_data_source_block           mn1299
_cod_depositor_comments
;

2020-11-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C30 H6 Cr2 F36 O12'
_cod_original_formula_weight         1346.35
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4318157
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.47221(3) 0.513496(19) 0.225077(12) 0.01464(7) Uani 1 1 d . . .
O1 O 0.47216(13) 0.37887(9) 0.17807(6) 0.0177(2) Uani 1 1 d . . .
O2 O 0.36143(13) 0.57506(9) 0.14452(6) 0.0193(2) Uani 1 1 d . . .
O3 O 0.58679(12) 0.45726(9) 0.30610(6) 0.0169(2) Uani 1 1 d . . .
O4 O 0.27744(13) 0.47747(9) 0.26728(6) 0.0178(2) Uani 1 1 d . . .
O5 O 0.66469(13) 0.55202(9) 0.18219(6) 0.0179(2) Uani 1 1 d . . .
O6 O 0.47110(13) 0.64394(9) 0.27622(6) 0.0180(2) Uani 1 1 d . . .
F1 F 0.33196(16) 0.18716(9) 0.14255(8) 0.0450(3) Uani 1 1 d . . .
F2 F 0.37276(17) 0.22365(10) 0.03469(7) 0.0445(3) Uani 1 1 d . . .
F3 F 0.56124(12) 0.20850(8) 0.10867(6) 0.0269(2) Uani 1 1 d . . .
F4 F 0.18447(16) 0.68439(10) 0.05990(6) 0.0405(3) Uani 1 1 d . . .
F5 F 0.1319(2) 0.55528(12) -0.00362(8) 0.0581(4) Uani 1 1 d . . .
F6 F 0.35025(18) 0.63022(16) -0.00974(9) 0.0749(7) Uani 1 1 d . . .
F7 F 0.59530(12) 0.38588(10) 0.48209(5) 0.0326(3) Uani 1 1 d . . .
F8 F 0.71990(13) 0.51429(9) 0.44007(6) 0.0315(2) Uani 1 1 d . . .
F9 F 0.76145(11) 0.35979(9) 0.40284(5) 0.0250(2) Uani 1 1 d . . .
F10 F -0.00409(12) 0.48416(10) 0.31085(6) 0.0343(3) Uani 1 1 d . . .
F11 F 0.06573(13) 0.33192(9) 0.34324(7) 0.0362(3) Uani 1 1 d . . .
F12 F 0.07391(12) 0.45822(11) 0.41699(6) 0.0349(3) Uani 1 1 d . . .
F13 F 0.97714(12) 0.55171(8) 0.16154(6) 0.0282(2) Uani 1 1 d . . .
F14 F 0.85219(13) 0.64969(10) 0.08865(5) 0.0305(2) Uani 1 1 d . . .
F15 F 0.98009(12) 0.71649(8) 0.17590(6) 0.0284(2) Uani 1 1 d . . .
F16 F 0.67168(12) 0.85528(8) 0.34513(6) 0.0264(2) Uani 1 1 d . . .
F17 F 0.54249(16) 0.74380(9) 0.40233(5) 0.0359(3) Uani 1 1 d . . .
F18 F 0.42850(12) 0.83968(8) 0.32419(6) 0.0287(2) Uani 1 1 d . . .
C1 C 0.40741(17) 0.35759(12) 0.11944(8) 0.0171(3) Uani 1 1 d . . .
C2 C 0.33035(19) 0.42451(13) 0.07339(8) 0.0209(3) Uani 1 1 d . . .
H2 H 0.2867 0.3988 0.0305 0.025 Uiso 1 1 calc R . .
C3 C 0.31653(17) 0.52879(13) 0.08949(8) 0.0180(3) Uani 1 1 d . . .
C4 C 0.41854(19) 0.24244(13) 0.10058(9) 0.0223(3) Uani 1 1 d . . .
C5 C 0.2452(2) 0.60095(14) 0.03298(9) 0.0243(3) Uani 1 1 d . . .
C6 C 0.53049(17) 0.44089(12) 0.36557(8) 0.0163(3) Uani 1 1 d . . .
C7 C 0.37736(18) 0.43823(13) 0.38234(8) 0.0186(3) Uani 1 1 d . . .
H7 H 0.3506 0.4263 0.4295 0.022 Uiso 1 1 calc R . .
C8 C 0.26203(17) 0.45295(12) 0.33063(8) 0.0172(3) Uani 1 1 d . . .
C9 C 0.65328(18) 0.42385(13) 0.42372(8) 0.0205(3) Uani 1 1 d . . .
C10 C 0.09600(18) 0.43237(14) 0.35078(9) 0.0212(3) Uani 1 1 d . . .
C11 C 0.74797(17) 0.62827(12) 0.19956(7) 0.0158(3) Uani 1 1 d . . .
C12 C 0.72146(18) 0.70324(12) 0.25008(8) 0.0179(3) Uani 1 1 d . . .
H12 H 0.7977 0.7536 0.2611 0.021 Uiso 1 1 calc R . .
C13 C 0.58382(17) 0.70459(11) 0.28442(8) 0.0158(3) Uani 1 1 d . . .
C14 C 0.89264(18) 0.63678(12) 0.15640(8) 0.0190(3) Uani 1 1 d . . .
C15 C 0.55723(19) 0.78793(12) 0.33971(8) 0.0198(3) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
O6 Cr1 O3 86.46(5) . . ?
O6 Cr1 O2 91.67(5) . . ?
O3 Cr1 O2 177.75(5) . . ?
O6 Cr1 O1 177.19(5) . . ?
O3 Cr1 O1 91.28(5) . . ?
O2 Cr1 O1 90.62(5) . . ?
O6 Cr1 O5 90.48(5) . . ?
O3 Cr1 O5 90.15(5) . . ?
O2 Cr1 O5 88.61(5) . . ?
O1 Cr1 O5 91.22(5) . . ?
O6 Cr1 O4 88.88(5) . . ?
O3 Cr1 O4 90.78(5) . . ?
O2 Cr1 O4 90.44(5) . . ?
O1 Cr1 O4 89.46(5) . . ?
O5 Cr1 O4 178.84(5) . . ?
C1 O1 Cr1 126.21(10) . . ?
C3 O2 Cr1 126.28(11) . . ?
C6 O3 Cr1 124.44(10) . . ?
C8 O4 Cr1 125.20(10) . . ?
C11 O5 Cr1 125.70(10) . . ?
C13 O6 Cr1 125.56(10) . . ?
O1 C1 C2 127.86(15) . . ?
O1 C1 C4 112.82(14) . . ?
C2 C1 C4 119.32(14) . . ?
C1 C2 C3 120.61(14) . . ?
O2 C3 C2 128.26(15) . . ?
O2 C3 C5 113.63(14) . . ?
C2 C3 C5 118.04(14) . . ?
F3 C4 F2 107.41(14) . . ?
F3 C4 F1 107.71(15) . . ?
F2 C4 F1 108.25(15) . . ?
F3 C4 C1 111.19(13) . . ?
F2 C4 C1 112.32(14) . . ?
F1 C4 C1 109.80(14) . . ?
F6 C5 F4 107.92(17) . . ?
F6 C5 F5 109.14(18) . . ?
F4 C5 F5 105.51(16) . . ?
F6 C5 C3 109.70(14) . . ?
F4 C5 C3 112.52(14) . . ?
F5 C5 C3 111.87(15) . . ?
O3 C6 C7 128.15(14) . . ?
O3 C6 C9 112.81(13) . . ?
C7 C6 C9 119.04(14) . . ?
C6 C7 C8 120.69(14) . . ?
O4 C8 C7 127.71(14) . . ?
O4 C8 C10 114.69(14) . . ?
C7 C8 C10 117.54(14) . . ?
F9 C9 F7 108.41(14) . . ?
F9 C9 F8 107.92(13) . . ?
F7 C9 F8 107.61(13) . . ?
F9 C9 C6 111.07(13) . . ?
F7 C9 C6 112.40(13) . . ?
F8 C9 C6 109.27(13) . . ?
F10 C10 F12 107.75(14) . . ?
F10 C10 F11 107.94(14) . . ?
F12 C10 F11 108.27(14) . . ?
F10 C10 C8 112.23(14) . . ?
F12 C10 C8 111.42(13) . . ?
F11 C10 C8 109.10(13) . . ?
O5 C11 C12 128.12(14) . . ?
O5 C11 C14 113.09(13) . . ?
C12 C11 C14 118.76(14) . . ?
C13 C12 C11 120.21(14) . . ?
O6 C13 C12 128.08(14) . . ?
O6 C13 C15 112.68(13) . . ?
C12 C13 C15 119.24(14) . . ?
F13 C14 F15 108.12(13) . . ?
F13 C14 F14 107.57(13) . . ?
F15 C14 F14 107.61(13) . . ?
F13 C14 C11 111.51(13) . . ?
F15 C14 C11 112.39(13) . . ?
F14 C14 C11 109.45(13) . . ?
F16 C15 F18 108.29(13) . . ?
F16 C15 F17 107.94(14) . . ?
F18 C15 F17 107.82(13) . . ?
F16 C15 C13 112.56(13) . . ?
F18 C15 C13 110.40(13) . . ?
F17 C15 C13 109.68(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 O6 1.9500(11) . ?
Cr1 O3 1.9513(11) . ?
Cr1 O2 1.9556(12) . ?
Cr1 O1 1.9594(11) . ?
Cr1 O5 1.9601(11) . ?
Cr1 O4 1.9638(12) . ?
O1 C1 1.2651(19) . ?
O2 C3 1.2586(19) . ?
O3 C6 1.2701(18) . ?
O4 C8 1.2610(19) . ?
O5 C11 1.2629(19) . ?
O6 C13 1.2641(19) . ?
F1 C4 1.330(2) . ?
F2 C4 1.328(2) . ?
F3 C4 1.325(2) . ?
F4 C5 1.315(2) . ?
F5 C5 1.329(2) . ?
F6 C5 1.305(2) . ?
F7 C9 1.3334(19) . ?
F8 C9 1.339(2) . ?
F9 C9 1.3286(19) . ?
F10 C10 1.321(2) . ?
F11 C10 1.333(2) . ?
F12 C10 1.3272(19) . ?
F13 C14 1.3270(19) . ?
F14 C14 1.3377(19) . ?
F15 C14 1.3287(19) . ?
F16 C15 1.3273(19) . ?
F17 C15 1.3344(19) . ?
F18 C15 1.3325(19) . ?
C1 C2 1.390(2) . ?
C1 C4 1.537(2) . ?
C2 C3 1.390(2) . ?
C3 C5 1.541(2) . ?
C6 C7 1.386(2) . ?
C6 C9 1.531(2) . ?
C7 C8 1.397(2) . ?
C8 C10 1.536(2) . ?
C11 C12 1.393(2) . ?
C11 C14 1.536(2) . ?
C12 C13 1.389(2) . ?
C13 C15 1.532(2) . ?
