#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/61/4076163.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_4076163
loop_
_publ_author_name
'Moriuchi, Akihiro'
'Uchida, Kazunori'
'Inagaki, Akiko'
'Akita, Munetaka'
_publ_section_title
;
 Photochromic Behavior and Diastereomeric Isomerism in
 [(η6-spirobenzopyran)RuCp*]PF6
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6382
_journal_paper_doi               10.1021/om0506771
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C31 H42 F6 N O1.5 P Ru'
_chemical_formula_weight         698.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 86.84(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.340(10)
_cell_length_b                   8.751(6)
_cell_length_c                   17.114(8)
_cell_measurement_reflns_used    11772
_cell_measurement_temperature    213.2
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      3.1
_cell_volume                     3042(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11417
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.85
_refine_diff_density_min         -1.96
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.468
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     413
_refine_ls_number_reflns         3536
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.0190
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2641
_reflns_number_gt                3536
_reflns_number_total             5857
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            om0506771si20051004_055427.cif
_cod_data_source_block           compound_3'b
_cod_original_cell_volume        3041(2)
_cod_original_formula_sum        'C31 H42 F6 N O1.50 P Ru '
_cod_database_code               4076163
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+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_calc_flag
_atom_site_refinement_flags
Ru(1) Ru -0.66981(3) 0.21064(8) 0.68908(4) 0.0523(3) Uani 1.00 d .
P(1) P -0.6869(2) -0.2765(3) 0.4663(2) 0.0708(7) Uani 1.00 d .
F(1) F -0.6939(5) -0.4523(8) 0.4765(5) 0.128(3) Uani 1.00 d .
F(2) F -0.7599(4) -0.250(1) 0.4966(6) 0.150(4) Uani 1.00 d .
F(3) F -0.6794(5) -0.0988(7) 0.4578(5) 0.138(3) Uani 1.00 d .
F(4) F -0.6122(4) -0.296(1) 0.4396(5) 0.122(3) Uani 1.00 d .
F(5) F -0.7065(4) -0.2887(8) 0.3790(4) 0.100(2) Uani 1.00 d .
F(6) F -0.6661(4) -0.2626(8) 0.5552(4) 0.107(2) Uani 1.00 d .
O(1) O -0.9004(7) 0.394(2) 0.7585(9) 0.078(4) Uani 0.59 d P
O(1A) O -0.902(1) 0.317(3) 0.788(1) 0.078(4) Uani 0.41 d P
O(2) O -1.024(2) 0.409(5) 0.457(3) 0.2032(2) Uiso 0.50 d P
N(1) N -0.7972(5) 0.460(1) 0.7259(6) 0.079(3) Uani 0.59 d P
N(1A) N -0.8033(5) 0.259(1) 0.8202(6) 0.077(3) Uani 0.41 d P
C(1) C -0.8363(4) 0.412(1) 0.7961(6) 0.078(3) Uani 1.00 d .
C(2) C -0.8413(6) 0.522(2) 0.8602(9) 0.135(7) Uani 1.00 d .
C(3) C -0.8983(7) 0.564(2) 0.896(1) 0.123(6) Uani 1.00 d .
C(4) C -0.9597(5) 0.510(1) 0.8688(8) 0.088(3) Uani 1.00 d .
C(5) C -1.0215(7) 0.551(2) 0.9006(9) 0.113(5) Uani 1.00 d .
C(6) C -1.0773(6) 0.508(2) 0.871(1) 0.132(7) Uani 1.00 d .
C(7) C -1.0747(6) 0.414(2) 0.809(1) 0.121(6) Uani 1.00 d .
C(8) C -1.0158(5) 0.362(2) 0.775(1) 0.111(5) Uani 1.00 d .
C(9) C -0.9589(5) 0.415(2) 0.8049(8) 0.093(4) Uani 1.00 d .
C(10) C -0.8033(5) 0.259(1) 0.8202(6) 0.077(3) Uani 0.59 d P
C(10A) C -0.7972(5) 0.460(1) 0.7259(6) 0.079(3) Uani 0.41 d P
C(11) C -0.7742(4) 0.206(1) 0.7444(6) 0.061(2) Uani 1.00 d .
C(12) C -0.7531(5) 0.056(1) 0.7251(7) 0.071(3) Uani 1.00 d .
C(13) C -0.7328(5) 0.032(1) 0.6457(8) 0.083(3) Uani 1.00 d .
C(14) C -0.7296(5) 0.146(2) 0.5927(6) 0.083(3) Uani 1.00 d .
C(15) C -0.7478(5) 0.295(1) 0.6148(6) 0.073(3) Uani 1.00 d .
C(16) C -0.7720(4) 0.322(1) 0.6897(6) 0.059(2) Uani 1.00 d .
C(17) C -0.863(1) 0.151(2) 0.854(2) 0.103(8) Uani 0.59 d P
C(17A) C -0.859(1) 0.521(3) 0.666(2) 0.079(8) Uani 0.41 d P
C(18) C -0.759(1) 0.296(3) 0.886(1) 0.091(7) Uani 0.59 d P
C(18A) C -0.756(1) 0.589(3) 0.746(2) 0.084(9) Uani 0.41 d P
C(19) C -0.800(1) 0.601(3) 0.678(2) 0.15(1) Uani 0.59 d P
C(19A) C -0.812(2) 0.149(5) 0.881(2) 0.11(1) Uani 0.41 d P
C(20) C -0.5818(4) 0.109(1) 0.7313(6) 0.061(2) Uani 1.00 d .
C(21) C -0.5956(4) 0.238(1) 0.7771(6) 0.068(3) Uani 1.00 d .
C(22) C -0.5945(4) 0.370(1) 0.7292(6) 0.061(2) Uani 1.00 d .
C(23) C -0.5770(4) 0.3163(10) 0.6510(6) 0.058(2) Uani 1.00 d .
C(24) C -0.5692(4) 0.155(1) 0.6521(6) 0.058(2) Uani 1.00 d .
C(25) C -0.5784(6) -0.056(1) 0.755(1) 0.119(6) Uani 1.00 d .
C(26) C -0.6031(7) 0.232(2) 0.8663(6) 0.124(6) Uani 1.00 d .
C(27) C -0.6016(6) 0.530(2) 0.754(1) 0.143(7) Uani 1.00 d .
C(28) C -0.5653(6) 0.421(1) 0.5820(7) 0.097(4) Uani 1.00 d .
C(29) C -0.5493(5) 0.058(1) 0.5829(7) 0.087(3) Uani 1.00 d .
C(31) C -0.966(3) 0.355(7) 0.498(4) 0.2242(3) Uiso 0.50 d P
C(32) C -0.929(2) 0.469(7) 0.534(3) 0.1873(2) Uiso 0.50 d P
C(33) C -0.955(5) 0.59(1) 0.473(8) 0.3150(5) Uiso 0.50 d P
C(34) C -0.995(4) 0.525(9) 0.438(4) 0.2087(3) Uiso 0.50 d P
H(1) H -0.8017 0.5647 0.8783 0.1511 Uiso 1.00 calc .
H(2) H -0.8976 0.6303 0.9418 0.1394 Uiso 1.00 calc .
H(3) H -1.0224 0.6206 0.9478 0.1351 Uiso 1.00 calc .
H(4) H -1.1191 0.5450 0.8944 0.1538 Uiso 1.00 calc .
H(5) H -1.1153 0.3830 0.7847 0.1408 Uiso 1.00 calc .
H(6) H -1.0148 0.2863 0.7340 0.1278 Uiso 1.00 calc .
H(7) H -0.7492 -0.0227 0.7646 0.0842 Uiso 1.00 calc .
H(8) H -0.7129 -0.0652 0.6312 0.0974 Uiso 1.00 calc .
H(9) H -0.7081 0.1317 0.5416 0.0999 Uiso 1.00 calc .
H(10) H -0.7389 0.3807 0.5784 0.0870 Uiso 1.00 calc .
H(11) H -0.6072 -0.1153 0.7245 0.1191 Uiso 1.00 calc .
H(12) H -0.5918 -0.0654 0.8096 0.1191 Uiso 1.00 calc .
H(13) H -0.5340 -0.0922 0.7466 0.1191 Uiso 1.00 calc .
H(14) H -0.6151 0.1300 0.8825 0.1237 Uiso 1.00 calc .
H(15) H -0.6367 0.3019 0.8847 0.1237 Uiso 1.00 calc .
H(16) H -0.5621 0.2591 0.8878 0.1237 Uiso 1.00 calc .
H(17) H -0.6225 0.5350 0.8054 0.1435 Uiso 1.00 calc .
H(18) H -0.6279 0.5840 0.7178 0.1435 Uiso 1.00 calc .
H(19) H -0.5588 0.5770 0.7541 0.1435 Uiso 1.00 calc .
H(20) H -0.5935 0.5089 0.5881 0.0972 Uiso 1.00 calc .
H(21) H -0.5748 0.3681 0.5348 0.0972 Uiso 1.00 calc .
H(22) H -0.5202 0.4539 0.5788 0.0972 Uiso 1.00 calc .
H(23) H -0.5723 0.0909 0.5384 0.0869 Uiso 1.00 calc .
H(24) H -0.5602 -0.0469 0.5943 0.0869 Uiso 1.00 calc .
H(25) H -0.5027 0.0669 0.5716 0.0869 Uiso 1.00 calc .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.102 0.094
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ru Ru -1.259 0.836
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
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
Ru(1) C(11) 2.277(9) . yes
Ru(1) C(12) 2.23(1) . yes
Ru(1) C(13) 2.18(1) . yes
Ru(1) C(14) 2.18(1) . yes
Ru(1) C(15) 2.21(1) . yes
Ru(1) C(16) 2.296(9) . yes
Ru(1) C(20) 2.160(9) . yes
Ru(1) C(21) 2.205(9) . yes
Ru(1) C(22) 2.206(9) . yes
Ru(1) C(23) 2.170(9) . yes
Ru(1) C(24) 2.163(8) . yes
P(1) F(1) 1.554(7) . yes
P(1) F(2) 1.563(9) . yes
P(1) F(3) 1.568(7) . yes
P(1) F(4) 1.571(8) . yes
P(1) F(5) 1.571(8) . yes
P(1) F(6) 1.606(8) . yes
O(1) O(1A) 0.84(3) . yes
O(1) C(1) 1.49(2) . yes
O(1) C(9) 1.41(2) . yes
O(1A) C(1) 1.58(3) . yes
O(1A) C(9) 1.46(3) . yes
O(2) C(31) 1.49(9) . yes
O(2) C(32) 1.42(7) 3_667 yes
O(2) C(33) 1.2(1) 3_667 yes
O(2) C(34) 1.22(9) . yes
N(1) C(1) 1.46(1) . yes
N(1) C(16) 1.44(1) . yes
N(1) C(17A) 1.74(3) . yes
N(1) C(18A) 1.46(3) . yes
N(1) C(19) 1.49(3) . yes
N(1A) C(1) 1.56(2) . yes
N(1A) C(11) 1.47(1) . yes
N(1A) C(17) 1.62(3) . yes
N(1A) C(18) 1.51(2) . yes
N(1A) C(19A) 1.42(4) . yes
C(1) C(2) 1.46(2) . yes
C(2) C(3) 1.33(2) . yes
C(3) C(4) 1.44(2) . yes
C(4) C(5) 1.39(2) . yes
C(4) C(9) 1.37(2) . yes
C(5) C(6) 1.33(2) . yes
C(6) C(7) 1.34(3) . yes
C(7) C(8) 1.38(2) . yes
C(8) C(9) 1.37(2) . yes
C(10) C(11) 1.47(1) . yes
C(10) C(17) 1.62(3) . yes
C(10) C(18) 1.51(2) . yes
C(10) C(19A) 1.42(4) . yes
C(10A) C(16) 1.44(1) . yes
C(10A) C(17A) 1.74(3) . yes
C(10A) C(18A) 1.46(3) . yes
C(10A) C(19) 1.49(3) . yes
C(11) C(12) 1.41(1) . yes
C(11) C(16) 1.38(1) . yes
C(12) C(13) 1.41(2) . yes
C(13) C(14) 1.35(2) . yes
C(14) C(15) 1.40(2) . yes
C(15) C(16) 1.37(1) . yes
C(17) C(19A) 1.15(4) . yes
C(17A) C(19) 1.40(4) . yes
C(18) C(19A) 1.69(4) . yes
C(18A) C(19) 1.51(5) . yes
C(20) C(21) 1.40(1) . yes
C(20) C(24) 1.42(1) . yes
C(20) C(25) 1.50(2) . yes
C(21) C(22) 1.41(1) . yes
C(21) C(26) 1.53(1) . yes
C(22) C(23) 1.44(1) . yes
C(22) C(27) 1.47(2) . yes
C(23) C(24) 1.42(1) . yes
C(23) C(28) 1.51(2) . yes
C(24) C(29) 1.50(2) . yes
C(31) C(32) 1.41(9) . yes
C(31) C(33) 1.7(1) 3_667 yes
C(31) C(34) 1.69(10) 3_667 yes
C(32) C(33) 1.6(1) . yes
C(32) C(34) 1.59(9) 3_667 yes
C(33) C(34) 1.2(1) . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
F(1) C(15) 3.38(1) 1_545
F(1) C(28) 3.44(2) 1_545
F(1) C(19A) 3.44(4) 4_445
F(1) C(26) 3.54(2) 4_445
F(2) C(19) 3.42(4) 1_545
F(2) C(2) 3.55(2) 4_455
F(3) C(14) 3.27(2) .
F(3) C(18) 3.37(2) 4_455
F(3) C(13) 3.53(2) .
F(4) C(25) 3.45(2) 4_445
F(5) C(18A) 3.08(3) 4_455
F(5) C(25) 3.54(2) 4_445
F(6) C(13) 3.27(1) .
F(6) C(28) 3.49(1) 1_545
F(6) C(19) 3.56(3) 1_545
O(2) C(17A) 3.32(6) 3_667
C(3) C(33) 3.5(1) 4_565
C(5) C(31) 3.19(7) 2_657
C(17) C(31) 3.14(7) 4_555
C(17) C(34) 3.34(8) 4_555
C(17) C(33) 3.4(1) 4_555
C(17) C(32) 3.46(6) 4_555
C(17A) C(32) 2.78(6) .
C(17A) C(34) 3.58(8) 3_667
C(29) C(29) 3.53(2) 3_656
