#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:28:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179482 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/79/4337910.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_4337910
loop_
_publ_author_name
'Phanopoulos, Andreas'
'Brown, Neil J.'
'White, Andrew J. P.'
'Long, Nicholas J.'
'Miller, Philip W.'
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of Ruthenium Hydride
 Complexes of N-Centered Triphosphine Ligands.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3742
_journal_paper_doi               10.1021/ic500030k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C43 H42 N P3 Ru'
_chemical_formula_sum            'C43 H42 N P3 Ru'
_chemical_formula_weight         766.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_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            6
_cell_length_a                   13.5997(2)
_cell_length_b                   13.5997(2)
_cell_length_c                   32.6601(7)
_cell_measurement_reflns_used    12374
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.6480
_cell_measurement_theta_min      3.0296
_cell_volume                     5231.27(16)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            18792
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         32.72
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0234
_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)+(0.0252P)²+8.7373P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                3624
_reflns_number_total             4008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500030k_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4337910--4337915.cif.
;
_cod_original_cell_volume        5231.3(2)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4337910
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
Ru1 Ru 0.6667 0.3333 0.044919(5) 0.01318(5) Uani 1 3 d S
N1 N 0.6667 0.3333 0.15071(5) 0.0177(3) Uani 1 3 d S
C2 C 0.55351(10) 0.31444(11) 0.14019(4) 0.0191(2) Uani 1 1 d .
H2A H 0.5349 0.3603 0.1588 0.023 Uiso 1 1 calc R
H2B H 0.4969 0.2335 0.1449 0.023 Uiso 1 1 calc R
P3 P 0.54079(3) 0.35189(3) 0.085826(9) 0.01455(6) Uani 1 1 d .
C4 C 0.55208(10) 0.49211(10) 0.09269(4) 0.0180(2) Uani 1 1 d .
C5 C 0.62700(11) 0.58459(11) 0.06912(4) 0.0205(2) Uani 1 1 d .
H5A H 0.6743 0.5762 0.0497 0.025 Uiso 1 1 calc R
C6 C 0.63349(13) 0.68988(12) 0.07371(5) 0.0273(3) Uani 1 1 d .
H6A H 0.6860 0.7527 0.0577 0.033 Uiso 1 1 calc R
C7 C 0.56403(15) 0.70307(13) 0.10132(5) 0.0330(3) Uani 1 1 d .
H7A H 0.5683 0.7746 0.1043 0.040 Uiso 1 1 calc R
C8 C 0.48805(16) 0.61112(14) 0.12463(6) 0.0386(4) Uani 1 1 d .
H8A H 0.4396 0.6196 0.1435 0.046 Uiso 1 1 calc R
C9 C 0.48216(14) 0.50676(13) 0.12066(5) 0.0306(3) Uani 1 1 d .
H9A H 0.4303 0.4446 0.1370 0.037 Uiso 1 1 calc R
C10 C 0.38662(10) 0.27379(10) 0.07592(4) 0.0166(2) Uani 1 1 d .
C11 C 0.30319(11) 0.19602(12) 0.10224(4) 0.0242(3) Uani 1 1 d .
H11A H 0.3246 0.1783 0.1277 0.029 Uiso 1 1 calc R
C12 C 0.18847(12) 0.14385(13) 0.09165(5) 0.0277(3) Uani 1 1 d .
H12A H 0.1325 0.0911 0.1099 0.033 Uiso 1 1 calc R
C13 C 0.15614(11) 0.16868(12) 0.05474(4) 0.0236(2) Uani 1 1 d .
H13A H 0.0781 0.1328 0.0475 0.028 Uiso 1 1 calc R
C14 C 0.23797(11) 0.24622(12) 0.02820(4) 0.0235(2) Uani 1 1 d .
H14A H 0.2159 0.2638 0.0029 0.028 Uiso 1 1 calc R
C15 C 0.35225(11) 0.29812(11) 0.03874(4) 0.0217(2) Uani 1 1 d .
H15A H 0.4078 0.3509 0.0204 0.026 Uiso 1 1 calc R
C21 C 0.6667 0.3333 -0.01891(6) 0.0219(4) Uani 1 3 d S
C22 C 0.56123(12) 0.23276(12) -0.00903(4) 0.0235(2) Uani 1 1 d .
H22A H 0.5559 0.1586 -0.0145 0.028 Uiso 1 1 calc R
H22B H 0.4903 0.2342 -0.0145 0.028 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'
N N 0.0061 0.0033 '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'
Ru Ru -1.2594 0.8363 '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
C21 Ru1 C22 38.51(4) . 2_655
C21 Ru1 C22 38.51(4) . .
C22 Ru1 C22 65.26(6) 2_655 .
C21 Ru1 C22 38.51(4) . 3_665
C22 Ru1 C22 65.26(6) 2_655 3_665
C22 Ru1 C22 65.26(6) . 3_665
C21 Ru1 P3 125.820(8) . 3_665
C22 Ru1 P3 99.93(4) 2_655 3_665
C22 Ru1 P3 164.01(4) . 3_665
C22 Ru1 P3 103.89(4) 3_665 3_665
C21 Ru1 P3 125.820(8) . 2_655
C22 Ru1 P3 103.89(4) 2_655 2_655
C22 Ru1 P3 99.93(4) . 2_655
C22 Ru1 P3 164.01(4) 3_665 2_655
P3 Ru1 P3 89.211(12) 3_665 2_655
C21 Ru1 P3 125.820(8) . .
C22 Ru1 P3 164.01(4) 2_655 .
C22 Ru1 P3 103.89(4) . .
C22 Ru1 P3 99.93(4) 3_665 .
P3 Ru1 P3 89.211(12) 3_665 .
P3 Ru1 P3 89.211(12) 2_655 .
C2 N1 C2 114.70(6) 2_655 3_665
C2 N1 C2 114.70(6) 2_655 .
C2 N1 C2 114.70(6) 3_665 .
N1 C2 P3 113.83(10) . .
C10 P3 C4 95.71(5) . .
C10 P3 C2 104.00(6) . .
C4 P3 C2 101.16(6) . .
C10 P3 Ru1 122.21(4) . .
C4 P3 Ru1 120.33(4) . .
C2 P3 Ru1 110.32(4) . .
C5 C4 C9 118.32(12) . .
C5 C4 P3 120.77(9) . .
C9 C4 P3 120.86(10) . .
C4 C5 C6 120.66(12) . .
C7 C6 C5 120.40(13) . .
C6 C7 C8 119.45(13) . .
C7 C8 C9 120.50(14) . .
C8 C9 C4 120.66(14) . .
C11 C10 C15 118.23(11) . .
C11 C10 P3 126.03(10) . .
C15 C10 P3 115.73(9) . .
C10 C11 C12 120.75(12) . .
C13 C12 C11 120.20(13) . .
C12 C13 C14 119.88(12) . .
C13 C14 C15 119.91(12) . .
C14 C15 C10 121.02(12) . .
C22 C21 C22 115.12(7) 2_655 .
C22 C21 C22 115.12(7) 2_655 3_665
C22 C21 C22 115.12(7) . 3_665
C22 C21 Ru1 77.03(10) 2_655 .
C22 C21 Ru1 77.03(10) . .
C22 C21 Ru1 77.03(10) 3_665 .
C21 C22 Ru1 64.46(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C21 2.085(2) .
Ru1 C22 2.2517(13) 2_655
Ru1 C22 2.2518(13) .
Ru1 C22 2.2517(13) 3_665
Ru1 P3 2.2828(3) 3_665
Ru1 P3 2.2828(3) 2_655
Ru1 P3 2.2828(3) .
N1 C2 1.4685(13) 2_655
N1 C2 1.4685(13) 3_665
N1 C2 1.4685(13) .
C2 P3 1.8788(12) .
P3 C10 1.8444(12) .
P3 C4 1.8486(12) .
C4 C5 1.3897(17) .
C4 C9 1.4027(18) .
C5 C6 1.3979(18) .
C6 C7 1.381(2) .
C7 C8 1.385(2) .
C8 C9 1.387(2) .
C10 C11 1.3946(17) .
C10 C15 1.3990(17) .
C11 C12 1.3965(19) .
C12 C13 1.382(2) .
C13 C14 1.3886(19) .
C14 C15 1.3911(18) .
C21 C22 1.4387(15) 2_655
C21 C22 1.4387(15) .
C21 C22 1.4387(15) 3_665
