#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/71/7117149.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_7117149
loop_
_publ_author_name
'Wenqing Wang'
'Xingyong Wang'
'Zaichao Zhang'
'Ningning Yuan'
'Xinping Wang'
_publ_section_title
;
 The long-sought seventeen-electron radical [(C6Me6)Cr(CO)3]+: isolation,
 crystal structure and substitution reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              8410
_journal_paper_doi               10.1039/C5cc01941A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C32 H33 Cr O2 P'
_chemical_formula_sum            'C32 H33 Cr O2 P'
_chemical_formula_weight         532.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-03 deposited with the CCDC.
2015-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.671(7)
_cell_angle_beta                 99.551(7)
_cell_angle_gamma                116.355(7)
_cell_formula_units_Z            2
_cell_length_a                   8.649(4)
_cell_length_b                   9.593(4)
_cell_length_c                   17.771(8)
_cell_measurement_reflns_used    3269
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.34
_cell_volume                     1296.8(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX DUO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.1143
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11036
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.838
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0832
_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)+(0.0905P)²+3.7366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2212
_reflns_number_gt                4166
_reflns_number_total             5799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01941a2.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_Hall     '-P 1  '
_cod_original_sg_symbol_H-M      'P -1  '
_cod_database_code               7117149
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.02549(9) 0.74677(7) 0.34448(4) 0.0154(2) Uani 1 1 d . . .
P1 P 0.06199(15) 0.74409(12) 0.21934(6) 0.0173(3) Uani 1 1 d . . .
C21 C 0.2625(6) 0.9014(5) 0.1956(3) 0.0195(9) Uani 1 1 d . . .
C5 C -0.1811(6) 0.8352(5) 0.3329(3) 0.0195(9) Uani 1 1 d . . .
C28 C -0.2806(6) 0.6266(5) 0.1377(3) 0.0255(10) Uani 1 1 d . . .
H28 H -0.3024 0.5462 0.1693 0.031 Uiso 1 1 calc R . .
C8 C 0.0693(6) 0.8518(5) 0.4626(2) 0.0188(9) Uani 1 1 d . . .
C3 C -0.0972(6) 0.7228(5) 0.4467(2) 0.0181(9) Uani 1 1 d . . .
C15 C 0.0796(6) 0.5734(4) 0.1789(3) 0.0199(9) Uani 1 1 d . . .
C2 C -0.0609(6) 0.5361(5) 0.3338(2) 0.0189(9) Uani 1 1 d . . .
C4 C -0.2223(6) 0.7127(5) 0.3809(3) 0.0199(9) Uani 1 1 d . . .
C27 C -0.1104(6) 0.7480(5) 0.1450(3) 0.0205(9) Uani 1 1 d . . .
C9 C -0.1515(7) 0.5961(5) 0.5013(3) 0.0275(11) Uani 1 1 d . . .
H9A H -0.0640 0.6283 0.5474 0.041 Uiso 1 1 calc R . .
H9B H -0.1627 0.5010 0.4774 0.041 Uiso 1 1 calc R . .
H9C H -0.2623 0.5789 0.5135 0.041 Uiso 1 1 calc R . .
C32 C -0.0817(7) 0.8690(5) 0.0973(3) 0.0227(10) Uani 1 1 d . . .
H32 H 0.0308 0.9506 0.1011 0.027 Uiso 1 1 calc R . .
C1 C 0.2441(6) 0.7646(5) 0.3730(3) 0.0229(10) Uani 1 1 d . . .
C31 C -0.2199(7) 0.8681(6) 0.0445(3) 0.0281(11) Uani 1 1 d . . .
H31 H -0.2003 0.9506 0.0142 0.034 Uiso 1 1 calc R . .
C10 C -0.4010(6) 0.5704(5) 0.3650(3) 0.0273(11) Uani 1 1 d . . .
H10A H -0.4796 0.5885 0.3914 0.041 Uiso 1 1 calc R . .
H10B H -0.3892 0.4808 0.3826 0.041 Uiso 1 1 calc R . .
H10C H -0.4472 0.5521 0.3109 0.041 Uiso 1 1 calc R . .
C13 C 0.2915(6) 1.1182(5) 0.4356(3) 0.0262(10) Uani 1 1 d . . .
H13A H 0.2969 1.1990 0.4032 0.039 Uiso 1 1 calc R . .
H13B H 0.3816 1.0888 0.4294 0.039 Uiso 1 1 calc R . .
H13C H 0.3091 1.1560 0.4881 0.039 Uiso 1 1 calc R . .
C7 C 0.1142(6) 0.9782(5) 0.4137(3) 0.0204(9) Uani 1 1 d . . .
C16 C 0.1963(6) 0.5264(5) 0.2219(3) 0.0237(10) Uani 1 1 d . . .
H16 H 0.2573 0.5771 0.2702 0.028 Uiso 1 1 calc R . .
C17 C 0.2215(7) 0.4060(5) 0.1932(3) 0.0269(11) Uani 1 1 d . . .
H17 H 0.3021 0.3783 0.2217 0.032 Uiso 1 1 calc R . .
C6 C -0.0126(6) 0.9677(5) 0.3492(3) 0.0205(9) Uani 1 1 d . . .
C14 C 0.2050(6) 0.8664(5) 0.5314(3) 0.0252(10) Uani 1 1 d . . .
H14A H 0.2016 0.9300 0.5726 0.038 Uiso 1 1 calc R . .
H14B H 0.3196 0.9139 0.5183 0.038 Uiso 1 1 calc R . .
H14C H 0.1804 0.7644 0.5472 0.038 Uiso 1 1 calc R . .
C11 C -0.3208(7) 0.8379(6) 0.2699(3) 0.0267(11) Uani 1 1 d . . .
H11A H -0.4075 0.7327 0.2522 0.040 Uiso 1 1 calc R . .
H11B H -0.2675 0.8883 0.2281 0.040 Uiso 1 1 calc R . .
H11C H -0.3760 0.8943 0.2895 0.040 Uiso 1 1 calc R . .
C24 C 0.5716(7) 1.1475(6) 0.1694(3) 0.0314(12) Uani 1 1 d . . .
H24 H 0.6750 1.2290 0.1605 0.038 Uiso 1 1 calc R . .
C25 C 0.4843(7) 1.0139(6) 0.1183(3) 0.0283(11) Uani 1 1 d . . .
H25 H 0.5287 1.0063 0.0750 0.034 Uiso 1 1 calc R . .
C23 C 0.5061(7) 1.1596(5) 0.2324(3) 0.0322(12) Uani 1 1 d . . .
H23 H 0.5633 1.2500 0.2662 0.039 Uiso 1 1 calc R . .
C22 C 0.3538(7) 1.0366(5) 0.2458(3) 0.0271(11) Uani 1 1 d . . .
H22 H 0.3115 1.0446 0.2896 0.033 Uiso 1 1 calc R . .
C30 C -0.3868(7) 0.7448(6) 0.0367(3) 0.0303(11) Uani 1 1 d . . .
H30 H -0.4781 0.7427 0.0000 0.036 Uiso 1 1 calc R . .
C26 C 0.3317(7) 0.8922(5) 0.1316(3) 0.0251(10) Uani 1 1 d . . .
H26 H 0.2743 0.8027 0.0973 0.030 Uiso 1 1 calc R . .
C29 C -0.4180(7) 0.6246(6) 0.0835(3) 0.0295(11) Uani 1 1 d . . .
H29 H -0.5306 0.5426 0.0788 0.035 Uiso 1 1 calc R . .
C12 C 0.0202(7) 1.1009(5) 0.2993(3) 0.0281(11) Uani 1 1 d . . .
H12A H -0.0614 1.1419 0.3035 0.042 Uiso 1 1 calc R . .
H12B H 0.0048 1.0636 0.2469 0.042 Uiso 1 1 calc R . .
H12C H 0.1381 1.1819 0.3159 0.042 Uiso 1 1 calc R . .
C20 C -0.0125(7) 0.4921(5) 0.1087(3) 0.0306(12) Uani 1 1 d . . .
H20 H -0.0922 0.5201 0.0795 0.037 Uiso 1 1 calc R . .
C19 C 0.0123(8) 0.3678(6) 0.0806(3) 0.0344(13) Uani 1 1 d . . .
H19 H -0.0510 0.3140 0.0330 0.041 Uiso 1 1 calc R . .
C18 C 0.1290(7) 0.3255(5) 0.1227(3) 0.0296(11) Uani 1 1 d . . .
H18 H 0.1459 0.2433 0.1041 0.035 Uiso 1 1 calc R . .
O2 O -0.1172(5) 0.3999(3) 0.3295(2) 0.0277(8) Uani 1 1 d . . .
O1 O 0.3863(5) 0.7801(4) 0.3971(2) 0.0327(8) 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'
O O 0.0106 0.0060 '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
C1 Cr1 C2 89.42(19) . .
C1 Cr1 C3 109.5(2) . .
C2 Cr1 C3 88.31(19) . .
C1 Cr1 C8 84.57(19) . .
C2 Cr1 C8 115.39(18) . .
C3 Cr1 C8 36.81(17) . .
C1 Cr1 C4 146.8(2) . .
C2 Cr1 C4 88.07(18) . .
C3 Cr1 C4 37.41(16) . .
C8 Cr1 C4 66.88(17) . .
C1 Cr1 C7 89.08(18) . .
C2 Cr1 C7 152.96(19) . .
C3 Cr1 C7 66.85(16) . .
C8 Cr1 C7 37.63(15) . .
C4 Cr1 C7 78.66(16) . .
C1 Cr1 C5 154.41(18) . .
C2 Cr1 C5 115.04(18) . .
C3 Cr1 C5 66.29(16) . .
C8 Cr1 C5 78.31(16) . .
C4 Cr1 C5 36.46(15) . .
C7 Cr1 C5 65.80(16) . .
C1 Cr1 C6 118.74(18) . .
C2 Cr1 C6 151.41(19) . .
C3 Cr1 C6 78.09(16) . .
C8 Cr1 C6 66.35(15) . .
C4 Cr1 C6 65.86(16) . .
C7 Cr1 C6 36.27(15) . .
C5 Cr1 C6 36.39(16) . .
C1 Cr1 P1 88.11(16) . .
C2 Cr1 P1 87.30(15) . .
C3 Cr1 P1 161.85(13) . .
C8 Cr1 P1 155.99(12) . .
C4 Cr1 P1 124.77(12) . .
C7 Cr1 P1 119.62(12) . .
C5 Cr1 P1 99.86(12) . .
C6 Cr1 P1 97.82(12) . .
C27 P1 C21 102.0(2) . .
C27 P1 C15 100.1(2) . .
C21 P1 C15 98.8(2) . .
C27 P1 Cr1 117.75(16) . .
C21 P1 Cr1 117.50(15) . .
C15 P1 Cr1 117.48(14) . .
C22 C21 C26 117.5(4) . .
C22 C21 P1 118.3(4) . .
C26 C21 P1 124.2(3) . .
C4 C5 C6 120.0(4) . .
C4 C5 C11 120.8(4) . .
C6 C5 C11 118.8(4) . .
C4 C5 Cr1 69.9(3) . .
C6 C5 Cr1 72.2(2) . .
C11 C5 Cr1 137.0(3) . .
C29 C28 C27 120.8(4) . .
C3 C8 C7 120.4(4) . .
C3 C8 C14 121.7(4) . .
C7 C8 C14 117.9(4) . .
C3 C8 Cr1 71.6(2) . .
C7 C8 Cr1 73.1(3) . .
C14 C8 Cr1 129.0(3) . .
C8 C3 C4 120.2(4) . .
C8 C3 C9 120.9(4) . .
C4 C3 C9 118.8(4) . .
C8 C3 Cr1 71.6(3) . .
C4 C3 Cr1 71.7(3) . .
C9 C3 Cr1 132.2(3) . .
C20 C15 C16 118.0(4) . .
C20 C15 P1 124.1(4) . .
C16 C15 P1 118.0(3) . .
O2 C2 Cr1 177.7(4) . .
C5 C4 C3 120.1(4) . .
C5 C4 C10 121.0(4) . .
C3 C4 C10 118.8(4) . .
C5 C4 Cr1 73.7(3) . .
C3 C4 Cr1 70.9(3) . .
C10 C4 Cr1 129.0(3) . .
C28 C27 C32 118.4(4) . .
C28 C27 P1 118.0(3) . .
C32 C27 P1 123.5(3) . .
C31 C32 C27 120.5(4) . .
O1 C1 Cr1 174.9(4) . .
C30 C31 C32 120.2(4) . .
C6 C7 C8 118.8(4) . .
C6 C7 C13 122.9(4) . .
C8 C7 C13 118.3(4) . .
C6 C7 Cr1 72.7(2) . .
C8 C7 Cr1 69.3(2) . .
C13 C7 Cr1 131.8(3) . .
C17 C16 C15 120.5(4) . .
C16 C17 C18 121.1(5) . .
C7 C6 C5 120.5(4) . .
C7 C6 C12 121.5(4) . .
C5 C6 C12 117.8(4) . .
C7 C6 Cr1 71.1(2) . .
C5 C6 Cr1 71.4(2) . .
C12 C6 Cr1 134.6(4) . .
C23 C24 C25 120.1(5) . .
C26 C25 C24 120.0(5) . .
C24 C23 C22 119.5(5) . .
C23 C22 C21 121.9(5) . .
C29 C30 C31 120.1(4) . .
C25 C26 C21 121.0(4) . .
C30 C29 C28 119.9(5) . .
C15 C20 C19 120.9(5) . .
C18 C19 C20 120.2(5) . .
C19 C18 C17 119.2(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 C1 1.804(5) .
Cr1 C2 1.812(4) .
Cr1 C3 2.217(5) .
Cr1 C8 2.216(4) .
Cr1 C4 2.228(5) .
Cr1 C7 2.267(4) .
Cr1 C5 2.277(4) .
Cr1 C6 2.288(4) .
Cr1 P1 2.2988(17) .
P1 C27 1.835(4) .
P1 C21 1.843(5) .
P1 C15 1.857(5) .
C21 C22 1.389(6) .
C21 C26 1.389(7) .
C5 C4 1.410(6) .
C5 C6 1.425(6) .
C5 C11 1.515(6) .
C28 C29 1.393(7) .
C28 C27 1.397(6) .
C8 C3 1.400(6) .
C8 C7 1.447(6) .
C8 C14 1.506(6) .
C3 C4 1.425(6) .
C3 C9 1.520(6) .
C15 C20 1.377(7) .
C15 C16 1.401(6) .
C2 O2 1.170(5) .
C4 C10 1.518(6) .
C27 C32 1.402(6) .
C32 C31 1.388(7) .
C1 O1 1.174(6) .
C31 C30 1.385(7) .
C13 C7 1.507(6) .
C7 C6 1.418(6) .
C16 C17 1.374(7) .
C17 C18 1.379(7) .
C6 C12 1.512(6) .
C24 C23 1.362(8) .
C24 C25 1.387(7) .
C25 C26 1.380(7) .
C23 C22 1.384(7) .
C30 C29 1.383(7) .
C20 C19 1.402(7) .
C19 C18 1.365(8) .
