#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/95/4329562.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_4329562
loop_
_publ_author_name
'Christopher C. Scarborough'
'Stephen Sproules'
'Christian J. Doonan'
'Karl S. Hagen'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_contact_author_address
;
Department of Chemistry
Emory University
Atlanta, GA 30322
;
_publ_contact_author_email       khagen@emory.edu
_publ_contact_author_fax         1-404-727-6586
_publ_contact_author_name        'Karl S. Hagen'
_publ_contact_author_phone       1-404-727-6556
_publ_section_title
;
 Scrutinizing Low-Spin Cr(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6969
_journal_page_last               6982
_journal_paper_doi               10.1021/ic300882r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C36 H24 Cr N6, 2.5(C2 H3 N), 2(F6 P)'
_chemical_formula_sum            'C41 H31.5 Cr F12 N8.5 P2'
_chemical_formula_weight         985.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   14.9676(11)
_cell_length_b                   14.9676(11)
_cell_length_c                   63.056(4)
_cell_measurement_temperature    100(2)
_cell_volume                     12233.8(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            29308
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.9220
_exptl_absorpt_correction_T_min  0.8823
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             5988
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.776
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6265
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.1069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0225P)²+279.8469P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2315
_refine_ls_wR_factor_ref         0.2415
_reflns_number_gt                4939
_reflns_number_total             6265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300882r_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C41 H31.50 Cr F12 N8.50 P2'
_cod_database_code               4329562
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 -0.3333 -0.6667 -0.01935(2) 0.0249(3) Uani 1 3 d S . .
N1 N -0.2717(3) -0.5311(3) -0.03597(6) 0.0252(9) Uani 1 1 d . . .
C2 C -0.3075(4) -0.5090(4) -0.05377(8) 0.0276(11) Uani 1 1 d . . .
H2 H -0.3661 -0.5629 -0.0607 0.033 Uiso 1 1 calc R . .
C3 C -0.2615(4) -0.4101(4) -0.06236(8) 0.0305(11) Uani 1 1 d . . .
H3 H -0.2881 -0.3975 -0.0750 0.037 Uiso 1 1 calc R . .
C4 C -0.1766(4) -0.3300(4) -0.05234(9) 0.0338(12) Uani 1 1 d . . .
H4 H -0.1452 -0.2621 -0.0580 0.041 Uiso 1 1 calc R . .
C5 C -0.1375(4) -0.3499(4) -0.03399(9) 0.0309(11) Uani 1 1 d . . .
C6 C -0.0498(4) -0.2722(5) -0.02212(10) 0.0414(14) Uani 1 1 d . . .
H6 H -0.0161 -0.2025 -0.0268 0.050 Uiso 1 1 calc R . .
C7 C -0.0154(5) -0.2972(5) -0.00460(11) 0.0447(15) Uani 1 1 d . . .
H7 H 0.0422 -0.2447 0.0028 0.054 Uiso 1 1 calc R . .
C8 C -0.0643(4) -0.4015(4) 0.00309(9) 0.0345(12) Uani 1 1 d . . .
C9 C -0.0309(4) -0.4324(5) 0.02104(9) 0.0384(13) Uani 1 1 d . . .
H9 H 0.0282 -0.3836 0.0287 0.046 Uiso 1 1 calc R . .
C10 C -0.0837(4) -0.5327(5) 0.02737(9) 0.0367(13) Uani 1 1 d . . .
H10 H -0.0624 -0.5540 0.0396 0.044 Uiso 1 1 calc R . .
C11 C -0.1695(4) -0.6047(5) 0.01572(8) 0.0336(12) Uani 1 1 d . . .
H11 H -0.2047 -0.6747 0.0202 0.040 Uiso 1 1 calc R . .
N12 N -0.2041(3) -0.5785(3) -0.00158(6) 0.0276(9) Uani 1 1 d . . .
C13 C -0.1506(4) -0.4781(4) -0.00784(8) 0.0282(11) Uani 1 1 d . . .
C14 C -0.1874(4) -0.4528(4) -0.02636(8) 0.0273(10) Uani 1 1 d . . .
Cr2 Cr 0.0000 0.0000 -0.15052(2) 0.0244(3) Uani 1 3 d S . .
N21 N -0.0751(3) -0.1354(3) -0.13390(6) 0.0280(9) Uani 1 1 d . . .
C22 C -0.0480(4) -0.1625(4) -0.11595(8) 0.0300(11) Uani 1 1 d . . .
H22 H 0.0109 -0.1114 -0.1086 0.036 Uiso 1 1 calc R . .
C23 C -0.1006(4) -0.2607(5) -0.10746(9) 0.0368(13) Uani 1 1 d . . .
H23 H -0.0779 -0.2760 -0.0946 0.044 Uiso 1 1 calc R . .
C24 C -0.1868(4) -0.3365(5) -0.11787(9) 0.0376(13) Uani 1 1 d . . .
H24 H -0.2226 -0.4048 -0.1124 0.045 Uiso 1 1 calc R . .
C25 C -0.2208(4) -0.3113(4) -0.13662(9) 0.0321(12) Uani 1 1 d . . .
C26 C -0.3080(5) -0.3829(5) -0.14880(10) 0.0397(14) Uani 1 1 d . . .
H26 H -0.3482 -0.4521 -0.1441 0.048 Uiso 1 1 calc R . .
C27 C -0.3348(4) -0.3533(5) -0.16721(10) 0.0379(13) Uani 1 1 d . . .
H27 H -0.3925 -0.4027 -0.1751 0.046 Uiso 1 1 calc R . .
C28 C -0.2769(4) -0.2492(4) -0.17468(8) 0.0330(12) Uani 1 1 d . . .
C29 C -0.3010(4) -0.2130(5) -0.19285(9) 0.0360(13) Uani 1 1 d . . .
H29 H -0.3579 -0.2590 -0.2014 0.043 Uiso 1 1 calc R . .
C30 C -0.2426(4) -0.1106(5) -0.19851(9) 0.0358(13) Uani 1 1 d . . .
H30 H -0.2601 -0.0852 -0.2107 0.043 Uiso 1 1 calc R . .
C31 C -0.1573(4) -0.0446(4) -0.18612(8) 0.0319(12) Uani 1 1 d . . .
H31 H -0.1169 0.0257 -0.1902 0.038 Uiso 1 1 calc R . .
N32 N -0.1302(3) -0.0773(3) -0.16860(7) 0.0273(9) Uani 1 1 d . . .
C33 C -0.1912(4) -0.1777(4) -0.16294(8) 0.0262(10) Uani 1 1 d . . .
C34 C -0.1616(4) -0.2088(4) -0.14396(8) 0.0264(10) Uani 1 1 d . . .
P40 P -0.00144(14) -0.47018(12) -0.09704(3) 0.0429(4) Uani 1 1 d . . .
F41 F -0.0845(5) -0.4712(4) -0.08106(10) 0.117(2) Uani 1 1 d . . .
F42 F 0.0716(4) -0.3507(3) -0.09317(7) 0.0748(15) Uani 1 1 d . . .
F43 F 0.0484(5) -0.4999(4) -0.07819(7) 0.101(2) Uani 1 1 d . . .
F44 F -0.0784(5) -0.5893(3) -0.10135(7) 0.0834(17) Uani 1 1 d . . .
F45 F -0.0543(4) -0.4451(4) -0.11655(8) 0.0745(14) Uani 1 1 d . . .
F46 F 0.0792(4) -0.4701(4) -0.11311(7) 0.0671(12) Uani 1 1 d . . .
P50 P 0.0000 0.0000 -0.05317(4) 0.0288(5) Uani 1 3 d S . .
F51 F 0.0806(3) -0.0134(3) -0.03857(6) 0.0450(9) Uani 1 1 d . . .
F52 F -0.0133(3) -0.0937(3) -0.06773(6) 0.0469(9) Uani 1 1 d . . .
N100 N 0.1875(6) -0.0782(6) -0.09407(13) 0.0515(19) Uani 0.708(9) 1 d PD A 1
C101 C 0.1877(14) -0.1201(12) -0.0795(2) 0.038(2) Uani 0.708(9) 1 d PD A 1
C102 C 0.1858(17) -0.1702(14) -0.0593(2) 0.055(3) Uani 0.708(9) 1 d PD A 1
H10A H 0.1752 -0.1334 -0.0476 0.082 Uiso 0.708(9) 1 calc PR A 1
H10B H 0.2515 -0.1686 -0.0573 0.082 Uiso 0.708(9) 1 calc PR A 1
H10C H 0.1294 -0.2420 -0.0595 0.082 Uiso 0.708(9) 1 calc PR A 1
N120 N -0.3333 -0.6667 -0.1499(4) 0.127(9) Uani 0.708(9) 3 d SPD A 1
C121 C -0.3333 -0.6667 -0.1321(4) 0.198(16) Uani 0.708(9) 3 d SPD A 1
C122 C -0.3333 -0.6667 -0.1091(4) 0.145(10) Uani 0.708(9) 3 d SPD A 1
N105 N 0.1862(15) -0.1965(15) -0.0412(3) 0.0515(19) Uani 0.292(9) 1 d PD A 2
C106 C 0.196(5) -0.158(4) -0.0571(6) 0.055(3) Uani 0.292(9) 1 d PD A 2
C107 C 0.195(4) -0.109(3) -0.0770(5) 0.038(2) Uani 0.292(9) 1 d PD A 2
H10D H 0.1871 -0.0489 -0.0741 0.058 Uiso 0.292(9) 1 calc PR A 2
H10E H 0.1365 -0.1587 -0.0857 0.058 Uiso 0.292(9) 1 calc PR A 2
H10F H 0.2593 -0.0872 -0.0847 0.058 Uiso 0.292(9) 1 calc PR A 2
N125 N -0.3333 -0.6667 -0.0902(6) 0.127(9) Uani 0.292(9) 3 d SPD A 2
C126 C -0.3333 -0.6667 -0.1080(6) 0.145(10) Uani 0.292(9) 3 d SPD A 2
C127 C -0.3333 -0.6667 -0.1310(6) 0.198(16) Uani 0.292(9) 3 d SPD A 2
N110 N 0.3333 -0.3333 -0.05306(19) 0.095(5) Uani 1 3 d S . .
C111 C 0.3333 -0.3333 -0.07123(18) 0.057(3) Uani 1 3 d S . .
C112 C 0.3333 -0.3333 -0.09420(19) 0.064(4) Uani 1 3 d S . .
H11A H 0.2662 -0.3876 -0.0994 0.097 Uiso 0.33 1 calc PR . .
H11B H 0.3876 -0.3462 -0.0994 0.097 Uiso 0.33 1 calc PR . .
H11C H 0.3462 -0.2662 -0.0994 0.097 Uiso 0.33 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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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
N12 Cr1 N12 92.87(17) 2_445 3_545
N12 Cr1 N12 92.87(17) 2_445 .
N12 Cr1 N12 92.87(17) 3_545 .
N12 Cr1 N1 172.11(17) 2_445 3_545
N12 Cr1 N1 80.16(17) 3_545 3_545
N12 Cr1 N1 91.19(16) . 3_545
N12 Cr1 N1 80.16(17) 2_445 2_445
N12 Cr1 N1 91.19(16) 3_545 2_445
N12 Cr1 N1 172.11(17) . 2_445
N1 Cr1 N1 96.17(15) 3_545 2_445
N12 Cr1 N1 91.19(16) 2_445 .
N12 Cr1 N1 172.11(17) 3_545 .
N12 Cr1 N1 80.17(17) . .
N1 Cr1 N1 96.17(15) 3_545 .
N1 Cr1 N1 96.17(15) 2_445 .
C2 N1 C14 117.9(4) . .
C2 N1 Cr1 129.0(3) . .
C14 N1 Cr1 112.9(3) . .
N1 C2 C3 122.5(5) . .
C4 C3 C2 119.5(5) . .
C3 C4 C5 119.6(5) . .
C4 C5 C14 117.6(5) . .
C4 C5 C6 124.3(5) . .
C14 C5 C6 118.1(5) . .
C7 C6 C5 121.1(6) . .
C6 C7 C8 121.4(5) . .
C9 C8 C13 117.3(5) . .
C9 C8 C7 123.9(5) . .
C13 C8 C7 118.8(5) . .
C10 C9 C8 119.6(5) . .
C9 C10 C11 119.8(5) . .
N12 C11 C10 122.6(5) . .
C11 N12 C13 117.1(4) . .
C11 N12 Cr1 129.3(4) . .
C13 N12 Cr1 113.5(3) . .
N12 C13 C8 123.5(5) . .
N12 C13 C14 116.1(4) . .
C8 C13 C14 120.4(5) . .
N1 C14 C5 122.9(5) . .
N1 C14 C13 116.8(5) . .
C5 C14 C13 120.3(5) . .
N32 Cr2 N32 91.95(17) 2 .
N32 Cr2 N32 91.95(17) 2 3
N32 Cr2 N32 91.95(17) . 3
N32 Cr2 N21 92.24(17) 2 .
N32 Cr2 N21 80.13(17) . .
N32 Cr2 N21 171.16(17) 3 .
N32 Cr2 N21 171.16(17) 2 3
N32 Cr2 N21 92.24(17) . 3
N32 Cr2 N21 80.13(17) 3 3
N21 Cr2 N21 96.14(16) . 3
N32 Cr2 N21 80.13(17) 2 2
N32 Cr2 N21 171.16(17) . 2
N32 Cr2 N21 92.24(17) 3 2
N21 Cr2 N21 96.14(16) . 2
N21 Cr2 N21 96.14(16) 3 2
C22 N21 C34 117.5(5) . .
C22 N21 Cr2 129.5(4) . .
C34 N21 Cr2 112.9(3) . .
N21 C22 C23 123.6(5) . .
C22 C23 C24 119.3(5) . .
C23 C24 C25 119.4(5) . .
C24 C25 C34 116.8(5) . .
C24 C25 C26 124.5(5) . .
C34 C25 C26 118.6(5) . .
C27 C26 C25 121.2(5) . .
C26 C27 C28 120.9(5) . .
C29 C28 C33 117.1(5) . .
C29 C28 C27 124.2(5) . .
C33 C28 C27 118.8(5) . .
C30 C29 C28 120.2(5) . .
C29 C30 C31 119.2(5) . .
N32 C31 C30 122.3(5) . .
C31 N32 C33 117.3(4) . .
C31 N32 Cr2 128.7(4) . .
C33 N32 Cr2 113.8(3) . .
N32 C33 C28 123.9(5) . .
N32 C33 C34 115.6(4) . .
C28 C33 C34 120.5(5) . .
N21 C34 C25 123.3(5) . .
N21 C34 C33 116.7(5) . .
C25 C34 C33 120.0(5) . .
F46 P40 F42 90.1(3) . .
F46 P40 F43 90.8(3) . .
F42 P40 F43 92.6(3) . .
F46 P40 F44 90.9(3) . .
F42 P40 F44 177.6(4) . .
F43 P40 F44 89.6(3) . .
F46 P40 F41 179.1(4) . .
F42 P40 F41 90.5(3) . .
F43 P40 F41 89.9(4) . .
F44 P40 F41 88.5(3) . .
F46 P40 F45 88.5(3) . .
F42 P40 F45 89.8(3) . .
F43 P40 F45 177.5(3) . .
F44 P40 F45 88.0(3) . .
F41 P40 F45 90.8(4) . .
F52 P50 F52 90.4(2) . 2
F52 P50 F52 90.4(2) . 3
F52 P50 F52 90.4(2) 2 3
F52 P50 F51 89.5(2) . .
F52 P50 F51 89.55(18) 2 .
F52 P50 F51 180.0(3) 3 .
F52 P50 F51 180.0(3) . 2
F52 P50 F51 89.5(2) 2 2
F52 P50 F51 89.55(18) 3 2
F51 P50 F51 90.5(2) . 2
F52 P50 F51 89.55(18) . 3
F52 P50 F51 180.0(3) 2 3
F52 P50 F51 89.5(2) 3 3
F51 P50 F51 90.5(2) . 3
F51 P50 F51 90.5(2) 2 3
N100 C101 C102 175(2) . .
N120 C121 C122 180.000(5) . .
N105 C106 C107 172(7) . .
N125 C126 C127 180.000(7) . .
N110 C111 C112 180.000(1) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N12 2.045(4) 2_445
Cr1 N12 2.045(4) 3_545
Cr1 N12 2.046(4) .
Cr1 N1 2.048(4) 3_545
Cr1 N1 2.048(4) 2_445
Cr1 N1 2.048(4) .
N1 C2 1.354(6) .
N1 C14 1.361(6) .
C2 C3 1.392(7) .
C3 C4 1.389(7) .
C4 C5 1.394(8) .
C5 C14 1.417(7) .
C5 C6 1.452(7) .
C6 C7 1.348(9) .
C7 C8 1.438(9) .
C8 C9 1.406(8) .
C8 C13 1.406(7) .
C9 C10 1.360(9) .
C10 C11 1.403(8) .
C11 N12 1.347(7) .
N12 C13 1.361(7) .
C13 C14 1.423(7) .
Cr2 N32 2.045(4) 2
Cr2 N32 2.045(4) .
Cr2 N32 2.045(4) 3
Cr2 N21 2.047(4) .
Cr2 N21 2.048(4) 3
Cr2 N21 2.048(4) 2
N21 C22 1.333(6) .
N21 C34 1.365(6) .
C22 C23 1.382(8) .
C23 C24 1.385(8) .
C24 C25 1.411(8) .
C25 C34 1.412(7) .
C25 C26 1.430(8) .
C26 C27 1.371(9) .
C27 C28 1.433(8) .
C28 C29 1.390(8) .
C28 C33 1.402(7) .
C29 C30 1.379(8) .
C30 C31 1.398(7) .
C31 N32 1.350(7) .
N32 C33 1.359(7) .
C33 C34 1.433(7) .
P40 F46 1.576(4) .
P40 F42 1.580(4) .
P40 F43 1.581(5) .
P40 F44 1.590(4) .
P40 F41 1.595(5) .
P40 F45 1.606(5) .
P50 F52 1.602(4) .
P50 F52 1.603(4) 2
P50 F52 1.603(4) 3
P50 F51 1.608(4) .
P50 F51 1.608(4) 2
P50 F51 1.608(4) 3
N100 C101 1.113(12) .
C101 C102 1.472(11) .
N120 C121 1.125(17) .
C121 C122 1.448(17) .
N105 C106 1.130(17) .
C106 C107 1.459(18) .
N125 C126 1.125(18) .
C126 C127 1.447(19) .
N110 C111 1.146(16) .
C111 C112 1.448(16) .
