#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011960.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_7011960
loop_
_publ_author_name
'Christopher J. Adams'
'Ian M. Bartlett'
'Neil G. Connelly'
'David J. Harding'
'Owen D. Hayward'
'Antonio J. Martín'
'A. Guy Orpen'
'Michael J. Quayle'
'Philip H. Rieger'
_publ_section_title
;
 Redox routes to arenechromium complexes of two-, three- and
 four-electron alkynes; structure and bonding in paramagnetic
 [Cr(CO)L(η-RCCR)(η-arene)]+
;
_journal_issue                   22
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4281
_journal_page_last               4288
_journal_paper_doi               10.1039/b206177p
_journal_year                    2002
_chemical_formula_sum            'C30 H32 Cr F6 O4 P'
_chemical_formula_weight         653.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9707(18)
_cell_length_b                   18.592(4)
_cell_length_c                   17.104(3)
_cell_measurement_reflns_used    197
_cell_measurement_temperature    293(2)
_cell_volume                     2831.4(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans with narrow frames'
_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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10012
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         3920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0574
_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)+(0.0546P)²+8.7062P] where 
P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                3157
_reflns_number_total             3920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206177p.txt
_cod_data_source_block           3plus
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7011960
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.23799(7) 0.74034(4) 0.49812(4) 0.0160(2) Uani 1 1 d . . .
C1 C 0.2851(5) 0.6617(2) 0.4021(3) 0.0210(11) Uani 1 1 d . . .
C2 C 0.1761(5) 0.6305(2) 0.4440(3) 0.0219(11) Uani 1 1 d . . .
C3 C 0.0422(5) 0.6696(2) 0.4549(3) 0.0203(10) Uani 1 1 d . . .
C4 C 0.0144(5) 0.7367(2) 0.4162(3) 0.0201(10) Uani 1 1 d . . .
C5 C 0.1231(5) 0.7684(2) 0.3736(3) 0.0188(10) Uani 1 1 d . . .
C6 C 0.2612(5) 0.7316(2) 0.3674(3) 0.0200(10) Uani 1 1 d . . .
C7 C 0.4261(6) 0.6200(3) 0.3920(3) 0.0302(12) Uani 1 1 d . . .
H7A H 0.4095 0.5913 0.3452 0.045 Uiso 1 1 calc R . .
H7B H 0.4514 0.5893 0.4368 0.045 Uiso 1 1 calc R . .
H7C H 0.5071 0.6530 0.3878 0.045 Uiso 1 1 calc R . .
C8 C 0.2042(6) 0.5555(3) 0.4779(3) 0.0305(12) Uani 1 1 d . . .
H8A H 0.1637 0.5205 0.4399 0.046 Uiso 1 1 calc R . .
H8B H 0.1563 0.5508 0.5248 0.046 Uiso 1 1 calc R . .
H8C H 0.3103 0.5479 0.4903 0.046 Uiso 1 1 calc R . .
C9 C -0.0752(5) 0.6366(3) 0.5010(3) 0.0260(11) Uani 1 1 d . . .
H9A H -0.1449 0.6089 0.4661 0.039 Uiso 1 1 calc R . .
H9B H -0.1282 0.6742 0.5245 0.039 Uiso 1 1 calc R . .
H9C H -0.0268 0.6059 0.5415 0.039 Uiso 1 1 calc R . .
C10 C -0.1330(5) 0.7743(3) 0.4224(3) 0.0317(12) Uani 1 1 d . . .
H10A H -0.2045 0.7612 0.3783 0.048 Uiso 1 1 calc R . .
H10B H -0.1179 0.8254 0.4225 0.048 Uiso 1 1 calc R . .
H10C H -0.1704 0.7602 0.4704 0.048 Uiso 1 1 calc R . .
C11 C 0.0871(5) 0.8388(2) 0.3314(3) 0.0215(11) Uani 1 1 d . . .
H11A H 0.0382 0.8295 0.2793 0.032 Uiso 1 1 calc R . .
H11B H 0.1783 0.8650 0.3281 0.032 Uiso 1 1 calc R . .
H11C H 0.0218 0.8667 0.3600 0.032 Uiso 1 1 calc R . .
C12 C 0.3748(6) 0.7611(3) 0.3173(3) 0.0259(11) Uani 1 1 d . . .
H12A H 0.3484 0.7463 0.2636 0.039 Uiso 1 1 calc R . .
H12B H 0.4728 0.7430 0.3363 0.039 Uiso 1 1 calc R . .
H12C H 0.3755 0.8126 0.3201 0.039 Uiso 1 1 calc R . .
C13 C 0.2407(5) 0.8481(2) 0.5179(3) 0.0183(10) Uani 1 1 d . . .
C21 C 0.2834(5) 0.9142(2) 0.4816(3) 0.0187(10) Uani 1 1 d . . .
C22 C 0.3997(5) 0.9181(2) 0.4345(3) 0.0197(10) Uani 1 1 d . . .
H22A H 0.4561 0.8771 0.4275 0.024 Uiso 1 1 calc R . .
C23 C 0.4333(5) 0.9816(2) 0.3979(3) 0.0215(11) Uani 1 1 d . . .
H23A H 0.5107 0.9831 0.3664 0.026 Uiso 1 1 calc R . .
C24 C 0.3505(5) 1.0427(2) 0.4086(3) 0.0228(11) Uani 1 1 d . . .
C25 C 0.2336(5) 1.0406(2) 0.4562(3) 0.0237(11) Uani 1 1 d . . .
H25A H 0.1780 1.0818 0.4633 0.028 Uiso 1 1 calc R . .
C26 C 0.2018(5) 0.9777(2) 0.4920(3) 0.0203(11) Uani 1 1 d . . .
H26A H 0.1250 0.9767 0.5239 0.024 Uiso 1 1 calc R . .
O3 O 0.3723(4) 1.10830(17) 0.3761(2) 0.0308(9) Uani 1 1 d . . .
C33 C 0.4819(6) 1.1138(3) 0.3224(3) 0.0359(14) Uani 1 1 d . . .
H33A H 0.4860 1.1625 0.3041 0.054 Uiso 1 1 calc R . .
H33B H 0.4550 1.0824 0.2784 0.054 Uiso 1 1 calc R . .
H33C H 0.5785 1.1002 0.3487 0.054 Uiso 1 1 calc R . .
C14 C 0.1660(5) 0.8196(2) 0.5688(3) 0.0182(10) Uani 1 1 d . . .
C27 C 0.0832(5) 0.8361(2) 0.6351(3) 0.0186(10) Uani 1 1 d . . .
C28 C -0.0232(5) 0.7893(2) 0.6614(3) 0.0206(11) Uani 1 1 d . . .
H28A H -0.0359 0.7436 0.6396 0.025 Uiso 1 1 calc R . .
C29 C -0.1091(5) 0.8101(3) 0.7191(3) 0.0204(11) Uani 1 1 d . . .
H29A H -0.1792 0.7785 0.7358 0.024 Uiso 1 1 calc R . .
C30 C -0.0910(5) 0.8779(3) 0.7520(3) 0.0207(11) Uani 1 1 d . . .
C31 C 0.0191(5) 0.9239(3) 0.7305(3) 0.0253(11) Uani 1 1 d . . .
H31A H 0.0348 0.9684 0.7549 0.030 Uiso 1 1 calc R . .
C32 C 0.1052(5) 0.9031(2) 0.6726(3) 0.0216(11) Uani 1 1 d . . .
H32A H 0.1789 0.9339 0.6584 0.026 Uiso 1 1 calc R . .
O4 O -0.1861(4) 0.89589(18) 0.80628(19) 0.0267(8) Uani 1 1 d . . .
C34 C -0.1974(6) 0.9710(3) 0.8242(3) 0.0340(13) Uani 1 1 d . . .
H34A H -0.2664 0.9773 0.8624 0.051 Uiso 1 1 calc R . .
H34B H -0.2331 0.9969 0.7771 0.051 Uiso 1 1 calc R . .
H34C H -0.1004 0.9890 0.8452 0.051 Uiso 1 1 calc R . .
C15 C 0.4498(5) 0.7494(2) 0.5171(3) 0.0203(11) Uani 1 1 d . . .
O1 O 0.5776(4) 0.75476(18) 0.5243(2) 0.0315(9) Uani 1 1 d . . .
C16 C 0.2299(5) 0.6922(2) 0.5932(3) 0.0205(11) Uani 1 1 d . . .
O2 O 0.2167(4) 0.66040(18) 0.6493(2) 0.0273(8) Uani 1 1 d . . .
P P 0.35919(14) 0.39693(7) 0.30522(8) 0.0247(3) Uani 1 1 d . . .
F1 F 0.2923(4) 0.47578(18) 0.2959(2) 0.0705(12) Uani 1 1 d . . .
F2 F 0.2016(4) 0.3669(2) 0.3262(2) 0.0596(10) Uani 1 1 d . . .
F3 F 0.3067(4) 0.38277(19) 0.21394(18) 0.0495(9) Uani 1 1 d . . .
F4 F 0.4278(4) 0.31797(16) 0.3148(2) 0.0510(9) Uani 1 1 d . . .
F5 F 0.4112(4) 0.41073(19) 0.3966(2) 0.0576(10) Uani 1 1 d . . .
F6 F 0.5160(3) 0.4253(2) 0.2839(2) 0.0573(10) 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'
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
_geom_angle_publ_flag
C16 Cr1 C15 92.21(19) . . ?
C16 Cr1 C13 109.21(19) . . ?
C15 Cr1 C13 83.80(18) . . ?
C16 Cr1 C14 77.51(19) . . ?
C15 Cr1 C14 102.43(18) . . ?
C13 Cr1 C14 36.34(18) . . ?
C16 Cr1 C3 83.91(18) . . ?
C15 Cr1 C3 146.69(18) . . ?
C13 Cr1 C3 128.72(17) . . ?
C14 Cr1 C3 108.90(17) . . ?
C16 Cr1 C6 147.12(18) . . ?
C15 Cr1 C6 87.98(18) . . ?
C13 Cr1 C6 103.50(17) . . ?
C14 Cr1 C6 134.45(17) . . ?
C3 Cr1 C6 78.23(16) . . ?
C16 Cr1 C1 110.53(18) . . ?
C15 Cr1 C1 84.87(18) . . ?
C13 Cr1 C1 138.96(18) . . ?
C14 Cr1 C1 169.16(18) . . ?
C3 Cr1 C1 65.95(17) . . ?
C6 Cr1 C1 36.72(16) . . ?
C16 Cr1 C2 83.72(18) . . ?
C15 Cr1 C2 109.77(18) . . ?
C13 Cr1 C2 161.33(18) . . ?
C14 Cr1 C2 143.16(17) . . ?
C3 Cr1 C2 36.95(17) . . ?
C6 Cr1 C2 65.46(16) . . ?
C1 Cr1 C2 35.90(17) . . ?
C16 Cr1 C4 113.10(18) . . ?
C15 Cr1 C4 152.49(18) . . ?
C13 Cr1 C4 97.05(17) . . ?
C14 Cr1 C4 93.80(17) . . ?
C3 Cr1 C4 36.32(17) . . ?
C6 Cr1 C4 65.00(16) . . ?
C1 Cr1 C4 76.49(17) . . ?
C2 Cr1 C4 64.92(17) . . ?
C16 Cr1 C5 148.39(18) . . ?
C15 Cr1 C5 117.57(18) . . ?
C13 Cr1 C5 85.78(17) . . ?
C14 Cr1 C5 104.08(17) . . ?
C3 Cr1 C5 65.50(16) . . ?
C6 Cr1 C5 36.32(16) . . ?
C1 Cr1 C5 65.21(16) . . ?
C2 Cr1 C5 76.62(16) . . ?
C4 Cr1 C5 35.73(16) . . ?
C2 C1 C6 120.4(4) . . ?
C2 C1 C7 119.4(4) . . ?
C6 C1 C7 120.2(4) . . ?
C2 C1 Cr1 72.3(3) . . ?
C6 C1 Cr1 71.6(2) . . ?
C7 C1 Cr1 130.0(3) . . ?
C1 C2 C3 120.1(4) . . ?
C1 C2 C8 118.7(4) . . ?
C3 C2 C8 121.2(4) . . ?
C1 C2 Cr1 71.8(3) . . ?
C3 C2 Cr1 70.1(3) . . ?
C8 C2 Cr1 130.2(3) . . ?
C4 C3 C2 119.1(4) . . ?
C4 C3 C9 120.2(4) . . ?
C2 C3 C9 120.4(4) . . ?
C4 C3 Cr1 74.0(3) . . ?
C2 C3 Cr1 72.9(3) . . ?
C9 C3 Cr1 129.0(3) . . ?
C5 C4 C3 120.9(4) . . ?
C5 C4 C10 120.5(4) . . ?
C3 C4 C10 118.6(4) . . ?
C5 C4 Cr1 72.4(3) . . ?
C3 C4 Cr1 69.6(3) . . ?
C10 C4 Cr1 130.4(3) . . ?
C4 C5 C6 119.8(4) . . ?
C4 C5 C11 119.1(4) . . ?
C6 C5 C11 121.1(4) . . ?
C4 C5 Cr1 71.9(3) . . ?
C6 C5 Cr1 70.5(2) . . ?
C11 C5 Cr1 132.9(3) . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C12 121.2(4) . . ?
C1 C6 C12 119.1(4) . . ?
C5 C6 Cr1 73.1(3) . . ?
C1 C6 Cr1 71.7(3) . . ?
C12 C6 Cr1 132.8(3) . . ?
C14 C13 C21 146.2(4) . . ?
C14 C13 Cr1 73.1(3) . . ?
C21 C13 Cr1 139.8(3) . . ?
C22 C21 C26 117.7(4) . . ?
C22 C21 C13 123.1(4) . . ?
C26 C21 C13 119.2(4) . . ?
C23 C22 C21 121.5(4) . . ?
C24 C23 C22 119.4(4) . . ?
O3 C24 C23 125.1(4) . . ?
O3 C24 C25 114.6(4) . . ?
C23 C24 C25 120.4(4) . . ?
C26 C25 C24 119.7(4) . . ?
C25 C26 C21 121.3(4) . . ?
C24 O3 C33 118.0(4) . . ?
C13 C14 C27 143.3(4) . . ?
C13 C14 Cr1 70.6(3) . . ?
C27 C14 Cr1 146.1(3) . . ?
C32 C27 C28 117.7(4) . . ?
C32 C27 C14 118.9(4) . . ?
C28 C27 C14 123.3(4) . . ?
C29 C28 C27 121.1(4) . . ?
C28 C29 C30 119.9(4) . . ?
O4 C30 C29 116.4(4) . . ?
O4 C30 C31 123.2(4) . . ?
C29 C30 C31 120.4(4) . . ?
C32 C31 C30 119.6(4) . . ?
C31 C32 C27 121.1(4) . . ?
C30 O4 C34 116.5(4) . . ?
O1 C15 Cr1 176.4(4) . . ?
O2 C16 Cr1 175.6(4) . . ?
F1 P F6 90.2(2) . . ?
F1 P F4 179.5(2) . . ?
F6 P F4 89.32(19) . . ?
F1 P F5 90.7(2) . . ?
F6 P F5 90.5(2) . . ?
F4 P F5 89.1(2) . . ?
F1 P F3 89.5(2) . . ?
F6 P F3 89.68(19) . . ?
F4 P F3 90.7(2) . . ?
F5 P F3 179.7(2) . . ?
F1 P F2 90.6(2) . . ?
F6 P F2 179.0(2) . . ?
F4 P F2 89.8(2) . . ?
F5 P F2 89.8(2) . . ?
F3 P F2 89.92(19) . . ?
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 C16 1.865(5) . ?
Cr1 C15 1.895(5) . ?
Cr1 C13 2.031(4) . ?
Cr1 C14 2.059(4) . ?
Cr1 C3 2.246(5) . ?
Cr1 C6 2.276(5) . ?
Cr1 C1 2.277(4) . ?
Cr1 C2 2.283(5) . ?
Cr1 C4 2.303(5) . ?
Cr1 C5 2.310(5) . ?
C1 C2 1.405(7) . ?
C1 C6 1.434(6) . ?
C1 C7 1.511(7) . ?
C2 C3 1.436(7) . ?
C2 C8 1.519(6) . ?
C3 C4 1.419(7) . ?
C3 C9 1.520(6) . ?
C4 C5 1.415(6) . ?
C4 C10 1.512(6) . ?
C5 C6 1.430(6) . ?
C5 C11 1.512(6) . ?
C6 C12 1.513(6) . ?
C13 C14 1.276(6) . ?
C13 C21 1.450(6) . ?
C21 C22 1.396(6) . ?
C21 C26 1.412(6) . ?
C22 C23 1.387(6) . ?
C23 C24 1.381(6) . ?
C24 O3 1.365(5) . ?
C24 C25 1.405(7) . ?
C25 C26 1.365(6) . ?
O3 C33 1.428(6) . ?
C14 C27 1.461(6) . ?
C27 C32 1.405(6) . ?
C27 C28 1.405(6) . ?
C28 C29 1.378(6) . ?
C29 C30 1.383(7) . ?
C30 O4 1.376(5) . ?
C30 C31 1.390(7) . ?
C31 C32 1.383(7) . ?
O4 C34 1.436(6) . ?
C15 O1 1.142(5) . ?
C16 O2 1.146(6) . ?
P F1 1.585(3) . ?
P F6 1.586(3) . ?
P F4 1.592(3) . ?
P F5 1.596(4) . ?
P F3 1.597(3) . ?
P F2 1.601(3) . ?
