#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:16:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179474 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/71/4337131.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_4337131
loop_
_publ_author_name
'Smart, Katharine A.'
'Grellier, Mary'
'Coppel, Yannick'
'Vendier, Laure'
'Mason, Sax A.'
'Capelli, Silvia C.'
'Albinati, Alberto'
'Montiel-Palma, Virginia'
'Muñoz-Hernández, Miguel A'
'Sabo-Etienne, Sylviane'
_publ_section_title
;
 Nature of si-h interactions in a series of ruthenium silazane complexes
 using multinuclear solid-state NMR and neutron diffraction.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1156
_journal_page_last               1165
_journal_paper_doi               10.1021/ic4027199
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H34 N2 Ru Si'
_chemical_formula_sum            'C25 H34 N2 Ru Si'
_chemical_formula_weight         491.7
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2660(11)
_cell_length_b                   15.8964(12)
_cell_length_c                   19.4635(15)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      34.55
_cell_measurement_theta_min      2.53
_cell_measurement_wavelength     0.71073
_cell_volume                     4413.9(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       ω-φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30437
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.48
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0265P)²+11.5071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                3616
_reflns_number_total             4480
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic4027199_si_002.cif
_cod_data_source_block           2b(mgo060308)
_cod_database_code               4337131
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -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
C1 C 0.7410(2) -0.1153(2) 0.24194(19) 0.0270(8) Uani 1 1 d .
H1A H 0.6969 -0.0739 0.2261 0.04 Uiso 1 1 calc R
H1B H 0.7155 -0.1441 0.2811 0.04 Uiso 1 1 calc R
H1C H 0.7529 -0.1551 0.2059 0.04 Uiso 1 1 calc R
C2 C 0.9314(3) -0.1517(2) 0.29556(19) 0.0267(8) Uani 1 1 d .
H2A H 0.9201 -0.1997 0.2667 0.04 Uiso 1 1 calc R
H2B H 0.9171 -0.1659 0.3424 0.04 Uiso 1 1 calc R
H2C H 0.996 -0.1356 0.2921 0.04 Uiso 1 1 calc R
C3 C 0.9126(2) -0.0816(2) 0.12102(17) 0.0239(7) Uani 1 1 d .
H3 H 0.9157 -0.1399 0.1187 0.029 Uiso 1 1 calc R
C4 C 0.9234(2) -0.0297(2) 0.06617(17) 0.0231(7) Uani 1 1 d .
H4 H 0.9351 -0.0459 0.0211 0.028 Uiso 1 1 calc R
C5 C 0.9135(2) 0.0544(2) 0.09095(16) 0.0197(7) Uani 1 1 d .
C6 C 0.8959(2) 0.0464(2) 0.16224(16) 0.0165(6) Uani 1 1 d .
C7 C 0.9166(2) 0.1359(2) 0.06510(17) 0.0241(8) Uani 1 1 d .
H7 H 0.9287 0.1459 0.0189 0.029 Uiso 1 1 calc R
C8 C 0.9011(2) 0.2017(2) 0.11036(17) 0.0252(8) Uani 1 1 d .
H8 H 0.9029 0.2568 0.0944 0.03 Uiso 1 1 calc R
C9 C 0.8827(2) 0.1861(2) 0.17954(16) 0.0197(7) Uani 1 1 d .
H9 H 0.8723 0.2319 0.2083 0.024 Uiso 1 1 calc R
C10 C 0.7463(2) 0.1594(2) 0.32111(17) 0.0239(8) Uani 1 1 d .
H10 H 0.7425 0.2 0.2834 0.029 Uiso 1 1 calc R
C11 C 0.7144(2) 0.0780(2) 0.30377(17) 0.0221(7) Uani 1 1 d .
H11 H 0.6931 0.0727 0.2561 0.027 Uiso 1 1 calc R
C12 C 0.6604(2) 0.0232(2) 0.35443(18) 0.0260(8) Uani 1 1 d .
H12A H 0.6165 -0.0115 0.329 0.031 Uiso 1 1 calc R
H12B H 0.6242 0.0594 0.3845 0.031 Uiso 1 1 calc R
C13 C 0.7225(2) -0.0344(2) 0.39883(17) 0.0237(8) Uani 1 1 d .
H13A H 0.6967 -0.037 0.4449 0.028 Uiso 1 1 calc R
H13B H 0.7215 -0.0908 0.3798 0.028 Uiso 1 1 calc R
C14 C 0.8235(2) -0.0037(2) 0.40258(16) 0.0190(7) Uani 1 1 d .
H14 H 0.8691 -0.0468 0.4161 0.023 Uiso 1 1 calc R
C15 C 0.8438(2) 0.0777(2) 0.42639(16) 0.0198(7) Uani 1 1 d .
H15 H 0.9015 0.0811 0.4536 0.024 Uiso 1 1 calc R
C16 C 0.7676(3) 0.1397(2) 0.44930(17) 0.0271(8) Uani 1 1 d .
H16A H 0.7143 0.1082 0.4665 0.032 Uiso 1 1 calc R
H16B H 0.7917 0.1736 0.4868 0.032 Uiso 1 1 calc R
C17 C 0.7346(3) 0.1981(2) 0.39180(19) 0.0302(9) Uani 1 1 d .
H17A H 0.669 0.2116 0.3989 0.036 Uiso 1 1 calc R
H17B H 0.7699 0.2501 0.3939 0.036 Uiso 1 1 calc R
C18 C 1.0220(2) 0.0408(2) 0.32629(16) 0.0215(7) Uani 1 1 d .
H18 H 1.0436 0.0054 0.2882 0.026 Uiso 1 1 calc R
C19 C 1.0123(2) 0.1248(2) 0.30694(16) 0.0224(8) Uani 1 1 d .
H19 H 1.0337 0.1393 0.2606 0.027 Uiso 1 1 calc R
C20 C 0.9714(2) 0.1908(2) 0.34570(18) 0.0248(8) Uani 1 1 d .
H20 H 0.9605 0.2424 0.3193 0.03 Uiso 1 1 calc R
C21 C 0.9912(3) 0.2055(2) 0.41854(19) 0.0330(9) Uani 1 1 d .
H21 H 0.9447 0.231 0.4447 0.04 Uiso 1 1 calc R
C22 C 1.0710(3) 0.1851(3) 0.4503(2) 0.0387(10) Uani 1 1 d .
H22 H 1.0752 0.1971 0.497 0.046 Uiso 1 1 calc R
C23 C 1.1543(3) 0.1445(3) 0.4171(2) 0.0428(11) Uani 1 1 d .
H23A H 1.2102 0.1625 0.4414 0.051 Uiso 1 1 calc R
H23B H 1.1591 0.1653 0.3704 0.051 Uiso 1 1 calc R
C24 C 1.1540(3) 0.0484(3) 0.41469(19) 0.0365(10) Uani 1 1 d .
H24A H 1.1729 0.0271 0.4593 0.044 Uiso 1 1 calc R
H24B H 1.2002 0.0299 0.3814 0.044 Uiso 1 1 calc R
C25 C 1.0588(2) 0.0099(3) 0.39581(18) 0.0264(8) Uani 1 1 d .
H25A H 1.0647 -0.0509 0.3945 0.032 Uiso 1 1 calc R
H25B H 1.0136 0.024 0.4312 0.032 Uiso 1 1 calc R
N2 N 0.89618(19) -0.03661(17) 0.18107(13) 0.0185(6) Uani 1 1 d .
N1 N 0.87926(17) 0.10834(17) 0.20724(13) 0.0165(6) Uani 1 1 d .
Si1 Si 0.85466(6) -0.06162(5) 0.26708(4) 0.01664(19) Uani 1 1 d .
Ru1 Ru 0.867741(16) 0.076260(16) 0.315542(12) 0.01321(8) 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 0 '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'
Si Si 0.0817 0.0704 '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
C4 C3 N2 111.6(3)
C3 C4 C5 106.9(3)
C7 C5 C6 116.4(3)
C7 C5 C4 138.3(3)
C6 C5 C4 105.3(3)
N1 C6 N2 122.3(3)
N1 C6 C5 127.3(3)
N2 C6 C5 110.4(3)
C8 C7 C5 117.9(3)
C7 C8 C9 120.6(3)
N1 C9 C8 123.8(3)
C11 C10 C17 123.6(3)
C11 C10 Ru1 71.91(18)
C17 C10 Ru1 112.3(2)
C10 C11 C12 122.1(3)
C10 C11 Ru1 70.49(19)
C12 C11 Ru1 115.3(2)
C11 C12 C13 114.3(3)
C14 C13 C12 112.4(3)
C15 C14 C13 120.3(3)
C15 C14 Ru1 70.37(18)
C13 C14 Ru1 114.7(2)
C14 C15 C16 122.8(3)
C14 C15 Ru1 72.34(18)
C16 C15 Ru1 113.9(2)
C17 C16 C15 113.3(3)
C10 C17 C16 112.6(3)
C19 C18 C25 125.4(3)
C19 C18 Ru1 69.05(18)
C25 C18 Ru1 119.4(2)
C18 C19 C20 127.3(3)
C18 C19 Ru1 74.80(19)
C20 C19 Ru1 80.45(19)
C19 C20 C21 123.6(3)
C19 C20 Ru1 64.21(18)
C21 C20 Ru1 118.2(2)
C22 C21 C20 125.1(4)
C21 C22 C23 125.5(4)
C22 C23 C24 116.2(3)
C23 C24 C25 114.1(3)
C18 C25 C24 112.7(3)
C6 N2 C3 105.7(3)
C6 N2 Si1 117.1(2)
C3 N2 Si1 135.7(2)
C6 N1 C9 113.9(3)
C6 N1 Ru1 118.3(2)
C9 N1 Ru1 127.2(2)
N2 Si1 C2 104.32(15)
N2 Si1 C1 98.01(15)
C2 Si1 C1 103.31(17)
N2 Si1 Ru1 97.88(9)
C2 Si1 Ru1 122.31(12)
C1 Si1 Ru1 125.48(12)
N1 Ru1 C10 88.06(11)
N1 Ru1 C15 165.15(12)
C10 Ru1 C15 79.66(13)
N1 Ru1 C11 88.35(11)
C10 Ru1 C11 37.60(13)
C15 Ru1 C11 86.99(12)
N1 Ru1 C19 76.94(11)
C10 Ru1 C19 122.26(14)
C15 Ru1 C19 102.54(12)
C11 Ru1 C19 156.40(13)
N1 Ru1 C14 154.07(11)
C10 Ru1 C14 94.81(13)
C15 Ru1 C14 37.29(12)
C11 Ru1 C14 78.66(12)
C19 Ru1 C14 121.71(12)
N1 Ru1 C18 94.24(10)
C10 Ru1 C18 155.68(13)
C15 Ru1 C18 93.60(12)
C11 Ru1 C18 166.41(13)
C19 Ru1 C18 36.15(13)
C14 Ru1 C18 93.60(12)
N1 Ru1 Si1 80.71(8)
C10 Ru1 Si1 120.82(10)
C15 Ru1 Si1 112.75(9)
C11 Ru1 Si1 83.86(10)
C19 Ru1 Si1 111.28(10)
C14 Ru1 Si1 75.70(9)
C18 Ru1 Si1 83.40(9)
N1 Ru1 C20 90.72(11)
C10 Ru1 C20 91.00(13)
C15 Ru1 C20 81.25(12)
C11 Ru1 C20 128.59(13)
C19 Ru1 C20 35.33(12)
C14 Ru1 C20 114.94(12)
C18 Ru1 C20 64.79(13)
Si1 Ru1 C20 146.41(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 Si1 1.897(4)
C2 Si1 1.886(4)
C3 C4 1.358(5)
C3 N2 1.390(4)
C4 C5 1.428(5)
C5 C7 1.391(5)
C5 C6 1.416(4)
C6 N1 1.339(4)
C6 N2 1.369(4)
C7 C8 1.385(5)
C8 C9 1.394(5)
C9 N1 1.349(4)
C10 C11 1.412(5)
C10 C17 1.517(5)
C10 Ru1 2.181(3)
C11 C12 1.525(5)
C11 Ru1 2.199(3)
C12 C13 1.539(5)
C13 C14 1.524(5)
C14 C15 1.405(5)
C14 Ru1 2.210(3)
C15 C16 1.534(5)
C15 Ru1 2.185(3)
C16 C17 1.528(5)
C18 C19 1.395(5)
C18 C25 1.532(4)
C18 Ru1 2.281(3)
C19 C20 1.418(5)
C19 Ru1 2.208(3)
C20 C21 1.464(5)
C20 Ru1 2.418(3)
C21 C22 1.335(6)
C22 C23 1.500(6)
C23 C24 1.528(6)
C24 C25 1.535(5)
N2 Si1 1.820(3)
N1 Ru1 2.175(3)
Si1 Ru1 2.3934(9)
