#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/66/4316682.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_4316682
loop_
_publ_author_name
'Gregorio Asensio'
'Ana B. Cuenca'
'Miguel A. Esteruelas'
'Mercedes Medio-Simón'
'Montserrat Oliván'
'Marta Valencia'
_publ_contact_author
;
  Dr. Montserrat Oliván
  Departamento de Química Inorgánica - I.C.M.A.
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       molivan@unizar.es
_publ_section_title
;
 Osmium(III) Complexes with POP Pincer Ligands: Preparation from
 Commercially Available OsCl3.3H2O and Their X-ray Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8665
_journal_page_last               8667
_journal_paper_doi               10.1021/ic101498h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C24 H34 O P2'
_chemical_formula_weight         400.45
_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
_cell_angle_alpha                104.497(5)
_cell_angle_beta                 96.286(5)
_cell_angle_gamma                103.323(5)
_cell_formula_units_Z            2
_cell_length_a                   7.398(2)
_cell_length_b                   10.020(3)
_cell_length_c                   16.463(5)
_cell_measurement_reflns_used    1451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1131.5(6)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'ω rotations 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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.1208
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10313
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         5340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0502
_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)+(0.0312P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                3207
_reflns_number_total             5340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101498h_si_002_2.cif
_cod_data_source_block           mae392as
_cod_database_code               4316682
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
P1 P 0.34412(9) 1.00245(7) 0.20008(4) 0.01936(16) Uani 1 1 d . . .
P2 P -0.04239(9) 0.52375(7) 0.34938(4) 0.02089(16) Uani 1 1 d . . .
O O 0.0433(2) 0.69159(15) 0.20050(9) 0.0171(4) Uani 1 1 d . . .
C1 C 0.5498(3) 0.9238(3) 0.19504(15) 0.0226(6) Uani 1 1 d . . .
H1 H 0.6488 0.9838 0.2455 0.027 Uiso 1 1 calc R . .
C2 C 0.6322(3) 0.9407(3) 0.11535(15) 0.0261(6) Uani 1 1 d . . .
H2A H 0.7436 0.9035 0.1134 0.039 Uiso 1 1 calc R . .
H2B H 0.6684 1.0421 0.1176 0.039 Uiso 1 1 calc R . .
H2C H 0.5372 0.8872 0.0642 0.039 Uiso 1 1 calc R . .
C3 C 0.5128(3) 0.7704(3) 0.19958(16) 0.0295(6) Uani 1 1 d . . .
H3A H 0.4196 0.7072 0.1500 0.044 Uiso 1 1 calc R . .
H3B H 0.4643 0.7637 0.2519 0.044 Uiso 1 1 calc R . .
H3C H 0.6307 0.7416 0.1998 0.044 Uiso 1 1 calc R . .
C4 C 0.2793(3) 0.9911(3) 0.30426(14) 0.0214(5) Uani 1 1 d . . .
H4 H 0.2667 0.8915 0.3082 0.026 Uiso 1 1 calc R . .
C5 C 0.4351(4) 1.0949(3) 0.37553(15) 0.0362(7) Uani 1 1 d . . .
H5A H 0.4567 1.1912 0.3685 0.054 Uiso 1 1 calc R . .
H5B H 0.5516 1.0644 0.3731 0.054 Uiso 1 1 calc R . .
H5C H 0.3971 1.0956 0.4308 0.054 Uiso 1 1 calc R . .
C6 C 0.0895(3) 1.0271(3) 0.31087(15) 0.0285(6) Uani 1 1 d . . .
H6A H 0.0584 1.0267 0.3672 0.043 Uiso 1 1 calc R . .
H6B H -0.0096 0.9555 0.2667 0.043 Uiso 1 1 calc R . .
H6C H 0.0985 1.1220 0.3029 0.043 Uiso 1 1 calc R . .
C7 C 0.1587(3) 0.8619(2) 0.12018(14) 0.0168(5) Uani 1 1 d . . .
C8 C 0.1267(3) 0.8837(2) 0.03938(14) 0.0202(5) Uani 1 1 d . . .
H8 H 0.2015 0.9677 0.0304 0.024 Uiso 1 1 calc R . .
C9 C -0.0089(3) 0.7886(2) -0.02819(14) 0.0214(6) Uani 1 1 d . . .
H9 H -0.0213 0.8075 -0.0820 0.026 Uiso 1 1 calc R . .
C10 C -0.1256(3) 0.6672(2) -0.01800(14) 0.0193(5) Uani 1 1 d . . .
H10 H -0.2197 0.6029 -0.0638 0.023 Uiso 1 1 calc R . .
C11 C -0.1014(3) 0.6416(2) 0.06144(14) 0.0160(5) Uani 1 1 d . . .
C12 C 0.0410(3) 0.7370(2) 0.12701(14) 0.0171(5) Uani 1 1 d . . .
C13 C -0.1035(3) 0.5671(2) 0.18112(14) 0.0168(5) Uani 1 1 d . . .
C14 C -0.1963(3) 0.5318(2) 0.09670(14) 0.0165(5) Uani 1 1 d . . .
C15 C -0.3501(3) 0.4112(2) 0.06580(15) 0.0197(5) Uani 1 1 d . . .
H15 H -0.4164 0.3854 0.0090 0.024 Uiso 1 1 calc R . .
C16 C -0.4033(3) 0.3303(2) 0.12029(15) 0.0208(5) Uani 1 1 d . . .
H16 H -0.5078 0.2478 0.1006 0.025 Uiso 1 1 calc R . .
C17 C -0.3066(3) 0.3676(2) 0.20339(15) 0.0204(5) Uani 1 1 d . . .
H17 H -0.3469 0.3085 0.2386 0.024 Uiso 1 1 calc R . .
C18 C -0.1522(3) 0.4885(2) 0.23782(14) 0.0170(5) Uani 1 1 d . . .
C19 C 0.2107(3) 0.5337(3) 0.34321(14) 0.0235(6) Uani 1 1 d . . .
H19 H 0.2779 0.6338 0.3458 0.028 Uiso 1 1 calc R . .
C20 C 0.2978(4) 0.4965(3) 0.42086(15) 0.0345(7) Uani 1 1 d . . .
H20A H 0.2358 0.3973 0.4179 0.052 Uiso 1 1 calc R . .
H20B H 0.2802 0.5608 0.4732 0.052 Uiso 1 1 calc R . .
H20C H 0.4330 0.5075 0.4211 0.052 Uiso 1 1 calc R . .
C21 C 0.2358(4) 0.4320(3) 0.26181(15) 0.0328(7) Uani 1 1 d . . .
H21A H 0.3685 0.4308 0.2655 0.049 Uiso 1 1 calc R . .
H21B H 0.1981 0.4646 0.2128 0.049 Uiso 1 1 calc R . .
H21C H 0.1568 0.3354 0.2548 0.049 Uiso 1 1 calc R . .
C22 C -0.0358(3) 0.7154(2) 0.39246(14) 0.0243(6) Uani 1 1 d . . .
H22 H 0.0086 0.7668 0.3505 0.029 Uiso 1 1 calc R . .
C23 C 0.1003(4) 0.7856(3) 0.47743(15) 0.0342(7) Uani 1 1 d . . .
H23A H 0.0962 0.8851 0.4993 0.051 Uiso 1 1 calc R . .
H23B H 0.2288 0.7835 0.4689 0.051 Uiso 1 1 calc R . .
H23C H 0.0632 0.7332 0.5185 0.051 Uiso 1 1 calc R . .
C24 C -0.2350(3) 0.7286(3) 0.40242(16) 0.0334(7) Uani 1 1 d . . .
H24A H -0.2750 0.6890 0.4483 0.050 Uiso 1 1 calc R . .
H24B H -0.3226 0.6757 0.3489 0.050 Uiso 1 1 calc R . .
H24C H -0.2346 0.8297 0.4165 0.050 Uiso 1 1 calc R . .
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'
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
C7 P1 C4 104.84(11) . . ?
C7 P1 C1 101.85(10) . . ?
C4 P1 C1 103.08(11) . . ?
C18 P2 C22 100.77(10) . . ?
C18 P2 C19 103.39(10) . . ?
C22 P2 C19 102.19(11) . . ?
C13 O C12 106.15(16) . . ?
C3 C1 C2 111.4(2) . . ?
C3 C1 P1 115.99(17) . . ?
C2 C1 P1 108.78(16) . . ?
C3 C1 H1 106.7 . . ?
C2 C1 H1 106.7 . . ?
P1 C1 H1 106.7 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C6 111.1(2) . . ?
C5 C4 P1 108.95(16) . . ?
C6 C4 P1 109.26(16) . . ?
C5 C4 H4 109.2 . . ?
C6 C4 H4 109.2 . . ?
P1 C4 H4 109.2 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 113.8(2) . . ?
C12 C7 P1 130.26(17) . . ?
C8 C7 P1 115.88(17) . . ?
C9 C8 C7 123.4(2) . . ?
C9 C8 H8 118.3 . . ?
C7 C8 H8 118.3 . . ?
C10 C9 C8 120.8(2) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 118.1(2) . . ?
C9 C10 H10 121.0 . . ?
C11 C10 H10 121.0 . . ?
C10 C11 C12 119.5(2) . . ?
C10 C11 C14 134.2(2) . . ?
C12 C11 C14 106.31(19) . . ?
C7 C12 O 125.0(2) . . ?
C7 C12 C11 124.3(2) . . ?
O C12 C11 110.61(19) . . ?
C18 C13 O 124.7(2) . . ?
C18 C13 C14 124.5(2) . . ?
O C13 C14 110.82(19) . . ?
C15 C14 C13 119.3(2) . . ?
C15 C14 C11 134.6(2) . . ?
C13 C14 C11 106.09(19) . . ?
C16 C15 C14 118.0(2) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C15 C16 C17 121.1(2) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C16 C17 C18 123.1(2) . . ?
C16 C17 H17 118.5 . . ?
C18 C17 H17 118.5 . . ?
C13 C18 C17 114.0(2) . . ?
C13 C18 P2 128.49(17) . . ?
C17 C18 P2 117.49(17) . . ?
C21 C19 C20 109.4(2) . . ?
C21 C19 P2 112.76(17) . . ?
C20 C19 P2 108.08(16) . . ?
C21 C19 H19 108.8 . . ?
C20 C19 H19 108.8 . . ?
P2 C19 H19 108.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C24 110.5(2) . . ?
C23 C22 P2 111.78(17) . . ?
C24 C22 P2 109.70(17) . . ?
C23 C22 H22 108.3 . . ?
C24 C22 H22 108.3 . . ?
P2 C22 H22 108.3 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
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
P1 C7 1.839(2) . ?
P1 C4 1.854(2) . ?
P1 C1 1.869(2) . ?
P2 C18 1.837(2) . ?
P2 C22 1.860(2) . ?
P2 C19 1.867(2) . ?
O C13 1.392(3) . ?
O C12 1.395(2) . ?
C1 C3 1.520(3) . ?
C1 C2 1.536(3) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.526(3) . ?
C4 C6 1.536(3) . ?
C4 H4 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C12 1.387(3) . ?
C7 C8 1.405(3) . ?
C8 C9 1.391(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.395(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.400(3) . ?
C11 C14 1.447(3) . ?
C13 C18 1.390(3) . ?
C13 C14 1.400(3) . ?
C14 C15 1.395(3) . ?
C15 C16 1.383(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.403(3) . ?
C17 H17 0.9500 . ?
C19 C21 1.525(3) . ?
C19 C20 1.535(3) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.529(3) . ?
C22 C24 1.532(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30661026
