#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:17:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179239 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/59/4315972.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_4315972
loop_
_publ_author_name
'Leslie D. Field'
'Hsiu L. Li'
'Scott J. Dalgarno'
_publ_section_title
;
 Side-on Bound Diazene and Hydrazine Complexes of Ruthenium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6214
_journal_page_last               6221
_journal_paper_doi               10.1021/ic100821u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C12 H32 N2 P4 Ru'
_chemical_formula_weight         429.35
_chemical_name_common            LHL2158
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.419(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6343(6)
_cell_length_b                   23.0314(16)
_cell_length_c                   9.3407(6)
_cell_measurement_reflns_used    8869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.73
_cell_volume                     1916.0(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14816
_diffrn_reflns_theta_full        30.44
_diffrn_reflns_theta_max         30.44
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.7254
_exptl_absorpt_correction_T_min  0.6577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2908
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0239P)²+2.8533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                2702
_reflns_number_total             2908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100821u_si_004.cif
_cod_data_source_block           LHL2158
_cod_database_code               4315972
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Ru1 Ru 0.5000 0.591418(7) 0.7500 0.01450(5) Uani 1 2 d S . .
P2 P 0.26725(5) 0.58866(2) 0.54887(5) 0.02554(10) Uani 0.33 1 d PD A 1
P4 P 0.38066(9) 0.65398(3) 0.85598(9) 0.01904(15) Uani 0.67 1 d PD A 2
N4 N 0.4528(2) 0.50295(7) 0.79321(18) 0.0311(3) Uani 1 1 d D . .
P1 P 0.5514(3) 0.65474(7) 0.5914(2) 0.0266(3) Uani 0.33 1 d PD A 1
C2 C 0.667(2) 0.6279(8) 0.485(2) 0.035(4) Uani 0.33 1 d PD A 1
H2A H 0.7196 0.6606 0.4615 0.053 Uiso 0.33 1 calc PR A 1
H2B H 0.6016 0.6093 0.3887 0.053 Uiso 0.33 1 calc PR A 1
H2C H 0.7402 0.5996 0.5496 0.053 Uiso 0.33 1 calc PR A 1
C6 C 0.1867(2) 0.51819(11) 0.4705(3) 0.0431(5) Uani 0.33 1 d PD A 1
H6A H 0.0784 0.5224 0.4124 0.065 Uiso 0.33 1 calc PR A 1
H6B H 0.2044 0.4907 0.5557 0.065 Uiso 0.33 1 calc PR A 1
H6C H 0.2340 0.5037 0.4014 0.065 Uiso 0.33 1 calc PR A 1
C8 C 0.1196(3) 0.62012(13) 0.6058(3) 0.0539(6) Uani 0.67 1 d PD A 2
H8A H 0.0337 0.6334 0.5133 0.065 Uiso 0.67 1 calc PR A 2
H8B H 0.0831 0.5909 0.6611 0.065 Uiso 0.67 1 calc PR A 2
C7 C 0.2414(3) 0.62664(14) 0.3684(3) 0.0604(8) Uani 0.67 1 d PD A 2
H7A H 0.3121 0.6112 0.3253 0.091 Uiso 0.67 1 calc PR A 2
H7B H 0.2600 0.6682 0.3893 0.091 Uiso 0.67 1 calc PR A 2
H7C H 0.1384 0.6208 0.2940 0.091 Uiso 0.67 1 calc PR A 2
C11 C 0.4472(5) 0.72797(17) 0.9294(6) 0.0537(11) Uani 0.67 1 d PD A 2
H11A H 0.4735 0.7491 0.8522 0.081 Uiso 0.67 1 calc PR A 2
H11B H 0.5359 0.7250 1.0260 0.081 Uiso 0.67 1 calc PR A 2
H11C H 0.3675 0.7488 0.9487 0.081 Uiso 0.67 1 calc PR A 2
C9 C 0.1935(4) 0.67264(16) 0.7147(4) 0.0456(8) Uani 0.67 1 d PD A 2
H9A H 0.1287 0.6845 0.7702 0.055 Uiso 0.67 1 calc PR A 2
H9B H 0.2016 0.7060 0.6514 0.055 Uiso 0.67 1 calc PR A 2
C3 C 0.3643(8) 0.6776(3) 0.4355(8) 0.0469(16) Uani 0.33 1 d PD A 1
H3A H 0.3201 0.7085 0.4788 0.056 Uiso 0.33 1 calc PR A 1
H3B H 0.3843 0.6948 0.3481 0.056 Uiso 0.33 1 calc PR A 1
C1 C 0.6298(10) 0.7281(3) 0.6460(8) 0.0408(18) Uani 0.33 1 d PD A 1
H1A H 0.7365 0.7252 0.7127 0.061 Uiso 0.33 1 calc PR A 1
H1B H 0.5759 0.7480 0.7019 0.061 Uiso 0.33 1 calc PR A 1
H1C H 0.6187 0.7500 0.5524 0.061 Uiso 0.33 1 calc PR A 1
C10 C 0.3479(11) 0.6323(4) 1.0298(10) 0.048(2) Uani 0.67 1 d PD A 2
H10A H 0.3330 0.6670 1.0830 0.072 Uiso 0.67 1 calc PR A 2
H10B H 0.4349 0.6106 1.0995 0.072 Uiso 0.67 1 calc PR A 2
H10C H 0.2582 0.6077 0.9997 0.072 Uiso 0.67 1 calc PR A 2
C4 C 0.2414(3) 0.62664(14) 0.3684(3) 0.0604(8) Uani 0.33 1 d PD A 1
H4A H 0.2645 0.6013 0.2947 0.073 Uiso 0.33 1 calc PR A 1
H4B H 0.1385 0.6424 0.3181 0.073 Uiso 0.33 1 calc PR A 1
C5 C 0.1196(3) 0.62012(13) 0.6058(3) 0.0539(6) Uani 0.33 1 d PD A 1
P3 P 0.26725(5) 0.58866(2) 0.54887(5) 0.02554(10) Uani 0.67 1 d PD A 2
C6A C 0.1867(2) 0.51819(11) 0.4705(3) 0.0431(5) Uani 0.67 1 d PD A 2
H6A1 H 0.0844 0.5237 0.3940 0.065 Uiso 0.67 1 calc PR A 2
H6A2 H 0.1840 0.4934 0.5547 0.065 Uiso 0.67 1 calc PR A 2
H6A3 H 0.2484 0.4997 0.4208 0.065 Uiso 0.67 1 calc PR A 2
H1N H 0.5181(10) 0.4968(11) 0.896(2) 0.052 Uiso 1 1 d 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'
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
_geom_angle_publ_flag
N4 Ru1 N4 38.61(9) 2_656 . ?
N4 Ru1 P1 111.80(6) 2_656 . ?
N4 Ru1 P1 147.61(6) . . ?
N4 Ru1 P1 147.61(6) 2_656 2_656 ?
N4 Ru1 P1 111.80(6) . 2_656 ?
P1 Ru1 P1 99.81(8) . 2_656 ?
N4 Ru1 P4 148.29(5) 2_656 . ?
N4 Ru1 P4 109.68(5) . . ?
P1 Ru1 P4 98.56(4) . . ?
P1 Ru1 P4 16.44(5) 2_656 . ?
N4 Ru1 P4 109.68(5) 2_656 2_656 ?
N4 Ru1 P4 148.29(5) . 2_656 ?
P1 Ru1 P4 16.44(5) . 2_656 ?
P1 Ru1 P4 98.56(4) 2_656 2_656 ?
P4 Ru1 P4 102.04(4) . 2_656 ?
N4 Ru1 P2 91.73(5) 2_656 . ?
N4 Ru1 P2 85.29(5) . . ?
P1 Ru1 P2 82.68(6) . . ?
P1 Ru1 P2 99.37(6) 2_656 . ?
P4 Ru1 P2 82.96(3) . . ?
P4 Ru1 P2 99.05(2) 2_656 . ?
N4 Ru1 P3 85.29(5) 2_656 2_656 ?
N4 Ru1 P3 91.73(5) . 2_656 ?
P1 Ru1 P3 99.37(6) . 2_656 ?
P1 Ru1 P3 82.68(6) 2_656 2_656 ?
P4 Ru1 P3 99.05(2) . 2_656 ?
P4 Ru1 P3 82.96(2) 2_656 2_656 ?
P2 Ru1 P3 176.85(2) . 2_656 ?
N4 Ru1 P2 85.29(5) 2_656 2_656 ?
N4 Ru1 P2 91.73(5) . 2_656 ?
P1 Ru1 P2 99.37(6) . 2_656 ?
P1 Ru1 P2 82.68(6) 2_656 2_656 ?
P4 Ru1 P2 99.05(2) . 2_656 ?
P4 Ru1 P2 82.96(2) 2_656 2_656 ?
P2 Ru1 P2 176.85(2) . 2_656 ?
P3 Ru1 P2 0.00(3) 2_656 2_656 ?
C6 P2 Ru1 118.82(8) . . ?
C9 P4 C10 104.3(3) . . ?
C9 P4 C11 99.0(2) . . ?
C10 P4 C11 94.3(3) . . ?
C9 P4 Ru1 110.75(11) . . ?
C10 P4 Ru1 119.6(3) . . ?
C11 P4 Ru1 125.25(13) . . ?
N4 N4 Ru1 70.69(4) 2_656 . ?
C1 P1 C2 100.8(7) . . ?
C1 P1 C3 97.3(4) . . ?
C2 P1 C3 105.6(6) . . ?
C1 P1 Ru1 125.4(2) . . ?
C2 P1 Ru1 117.4(6) . . ?
C3 P1 Ru1 107.3(2) . . ?
C8 C9 P4 111.4(2) . . ?
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
Ru1 N4 2.1589(15) 2_656 ?
Ru1 N4 2.1589(15) . ?
Ru1 P1 2.2642(16) . ?
Ru1 P1 2.2642(15) 2_656 ?
Ru1 P4 2.2904(8) . ?
Ru1 P4 2.2904(8) 2_656 ?
Ru1 P2 2.3127(4) . ?
Ru1 P3 2.3127(4) 2_656 ?
Ru1 P2 2.3127(4) 2_656 ?
P2 C6 1.827(2) . ?
P4 C9 1.834(3) . ?
P4 C10 1.838(7) . ?
P4 C11 1.858(4) . ?
N4 N4 1.427(3) 2_656 ?
P1 C1 1.841(6) . ?
P1 C2 1.855(14) . ?
P1 C3 1.910(7) . ?
C8 C9 1.566(5) . ?
