#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:07:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179741 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/37/7003710.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_7003710
loop_
_publ_author_name
'Lee, Kajin'
'Clark, Timothy J.'
'Lough, Alan J.'
'Manners, Ian'
_publ_section_title
;
 Synthesis and dehydrocoupling reactivity of iron and ruthenium
 phosphine--borane complexes
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              2732
_journal_page_last               2740
_journal_paper_doi               10.1039/b718918d
_journal_year                    2008
_chemical_formula_moiety         'C19 H18 B O2 P Ru'
_chemical_formula_sum            'C19 H18 B O2 P Ru'
_chemical_formula_weight         421.18
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.7740(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4151(5)
_cell_length_b                   9.7058(3)
_cell_length_c                   14.0420(5)
_cell_measurement_reflns_used    11118
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1789.86(11)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'SHELXTL V6.1'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11118
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.730
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0.0033(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0439P)²+5.4157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                3156
_reflns_number_total             4085
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b718918d.txt
_cod_data_source_block           k0680
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7003710
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.60195(2) 0.60084(3) 0.38664(2) 0.02098(14) Uani 1 1 d . . .
P1 P 0.54061(8) 0.68574(11) 0.22671(7) 0.0206(2) Uani 1 1 d . . .
O1 O 0.4405(3) 0.3791(3) 0.3437(2) 0.0340(7) Uani 1 1 d . . .
O2 O 0.4578(3) 0.7815(4) 0.4708(2) 0.0396(8) Uani 1 1 d . . .
C1 C 0.7280(4) 0.5508(7) 0.5147(4) 0.0494(15) Uani 1 1 d . . .
H1A H 0.7196 0.5279 0.5820 0.059 Uiso 1 1 calc R . .
C2 C 0.7451(4) 0.6830(6) 0.4796(5) 0.0520(16) Uani 1 1 d . . .
H2A H 0.7511 0.7703 0.5181 0.062 Uiso 1 1 calc R . .
C3 C 0.7607(3) 0.6700(6) 0.3846(4) 0.0453(14) Uani 1 1 d . . .
H3A H 0.7803 0.7456 0.3437 0.054 Uiso 1 1 calc R . .
C4 C 0.7523(3) 0.5288(6) 0.3602(4) 0.0399(12) Uani 1 1 d . . .
H4A H 0.7647 0.4870 0.2986 0.048 Uiso 1 1 calc R . .
C5 C 0.7328(4) 0.4567(6) 0.4405(4) 0.0418(12) Uani 1 1 d . . .
H5A H 0.7279 0.3542 0.4455 0.050 Uiso 1 1 calc R . .
C6 C 0.5012(3) 0.4643(5) 0.3593(3) 0.0261(9) Uani 1 1 d . . .
C7 C 0.5114(3) 0.7148(4) 0.4371(3) 0.0256(9) Uani 1 1 d . . .
C8 C 0.4075(3) 0.6316(4) 0.1870(3) 0.0217(8) Uani 1 1 d . . .
C9 C 0.3825(3) 0.5276(5) 0.1180(3) 0.0289(9) Uani 1 1 d . . .
H9A H 0.4331 0.4910 0.0866 0.035 Uiso 1 1 calc R . .
C10 C 0.2831(4) 0.4771(5) 0.0948(4) 0.0393(12) Uani 1 1 d . . .
H10A H 0.2664 0.4059 0.0477 0.047 Uiso 1 1 calc R . .
C11 C 0.2091(4) 0.5298(5) 0.1397(4) 0.0374(11) Uani 1 1 d . . .
H11A H 0.1418 0.4942 0.1240 0.045 Uiso 1 1 calc R . .
C12 C 0.2325(3) 0.6343(5) 0.2075(4) 0.0341(11) Uani 1 1 d . . .
H12A H 0.1814 0.6709 0.2382 0.041 Uiso 1 1 calc R . .
C13 C 0.3316(3) 0.6857(5) 0.2307(3) 0.0275(9) Uani 1 1 d . . .
H13A H 0.3475 0.7583 0.2766 0.033 Uiso 1 1 calc R . .
C14 C 0.5302(3) 0.8754(4) 0.2220(3) 0.0227(8) Uani 1 1 d . . .
C15 C 0.5714(3) 0.9624(4) 0.2989(3) 0.0247(9) Uani 1 1 d . . .
H15A H 0.6040 0.9242 0.3596 0.030 Uiso 1 1 calc R . .
C16 C 0.5653(3) 1.1023(5) 0.2878(3) 0.0320(10) Uani 1 1 d . . .
H16A H 0.5941 1.1605 0.3406 0.038 Uiso 1 1 calc R . .
C17 C 0.5177(3) 1.1595(5) 0.2007(4) 0.0319(10) Uani 1 1 d . . .
H17A H 0.5136 1.2568 0.1936 0.038 Uiso 1 1 calc R . .
C18 C 0.4757(3) 1.0752(5) 0.1232(3) 0.0297(10) Uani 1 1 d . . .
H18A H 0.4425 1.1145 0.0631 0.036 Uiso 1 1 calc R . .
C19 C 0.4821(3) 0.9338(5) 0.1337(3) 0.0280(9) Uani 1 1 d . . .
H19A H 0.4536 0.8759 0.0805 0.034 Uiso 1 1 calc R . .
B1 B 0.6201(4) 0.6296(6) 0.1302(4) 0.0298(11) Uani 1 1 d . . .
H1 H 0.575(4) 0.672(5) 0.059(4) 0.034(13) Uiso 1 1 d . . .
H2 H 0.696(4) 0.669(6) 0.157(4) 0.047(15) Uiso 1 1 d . . .
H3 H 0.619(4) 0.526(6) 0.130(4) 0.039(14) Uiso 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 0.0000 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'
Ru Ru -1.2594 0.8363 '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'
B B 0.0013 0.0007 '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
C6 Ru1 C7 89.95(18) . . ?
C6 Ru1 C4 112.44(19) . . ?
C7 Ru1 C4 156.7(2) . . ?
C6 Ru1 C2 150.2(2) . . ?
C7 Ru1 C2 96.53(19) . . ?
C4 Ru1 C2 60.8(2) . . ?
C6 Ru1 C3 149.0(2) . . ?
C7 Ru1 C3 121.1(2) . . ?
C4 Ru1 C3 36.8(2) . . ?
C2 Ru1 C3 36.4(2) . . ?
C6 Ru1 C5 96.28(19) . . ?
C7 Ru1 C5 139.18(19) . . ?
C4 Ru1 C5 36.25(19) . . ?
C2 Ru1 C5 60.5(2) . . ?
C3 Ru1 C5 60.8(2) . . ?
C6 Ru1 C1 113.7(2) . . ?
C7 Ru1 C1 105.21(19) . . ?
C4 Ru1 C1 60.69(18) . . ?
C2 Ru1 C1 36.6(2) . . ?
C3 Ru1 C1 60.9(2) . . ?
C5 Ru1 C1 36.1(2) . . ?
C6 Ru1 P1 87.47(13) . . ?
C7 Ru1 P1 91.51(12) . . ?
C4 Ru1 P1 95.83(13) . . ?
C2 Ru1 P1 121.21(19) . . ?
C3 Ru1 P1 91.78(15) . . ?
C5 Ru1 P1 128.95(15) . . ?
C1 Ru1 P1 152.49(15) . . ?
C8 P1 C14 102.28(19) . . ?
C8 P1 B1 110.0(2) . . ?
C14 P1 B1 107.4(2) . . ?
C8 P1 Ru1 108.40(13) . . ?
C14 P1 Ru1 112.87(14) . . ?
B1 P1 Ru1 115.06(17) . . ?
C5 C1 C2 107.3(5) . . ?
C5 C1 Ru1 71.8(3) . . ?
C2 C1 Ru1 71.0(3) . . ?
C3 C2 C1 108.6(5) . . ?
C3 C2 Ru1 71.9(3) . . ?
C1 C2 Ru1 72.4(3) . . ?
C2 C3 C4 107.5(5) . . ?
C2 C3 Ru1 71.8(3) . . ?
C4 C3 Ru1 71.5(3) . . ?
C5 C4 C3 108.0(5) . . ?
C5 C4 Ru1 72.5(3) . . ?
C3 C4 Ru1 71.7(3) . . ?
C4 C5 C1 108.6(5) . . ?
C4 C5 Ru1 71.2(3) . . ?
C1 C5 Ru1 72.1(3) . . ?
O1 C6 Ru1 178.8(4) . . ?
O2 C7 Ru1 177.5(4) . . ?
C9 C8 C13 119.0(4) . . ?
C9 C8 P1 120.0(3) . . ?
C13 C8 P1 120.8(3) . . ?
C8 C9 C10 120.0(4) . . ?
C11 C10 C9 120.4(4) . . ?
C10 C11 C12 120.2(4) . . ?
C11 C12 C13 119.6(4) . . ?
C12 C13 C8 120.7(4) . . ?
C15 C14 C19 118.7(4) . . ?
C15 C14 P1 124.2(3) . . ?
C19 C14 P1 117.0(3) . . ?
C16 C15 C14 120.5(4) . . ?
C15 C16 C17 120.6(4) . . ?
C16 C17 C18 120.0(4) . . ?
C19 C18 C17 119.8(4) . . ?
C18 C19 C14 120.4(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
Ru1 C6 1.875(5) . ?
Ru1 C7 1.885(4) . ?
Ru1 C4 2.235(4) . ?
Ru1 C2 2.237(5) . ?
Ru1 C3 2.238(5) . ?
Ru1 C5 2.252(5) . ?
Ru1 C1 2.255(5) . ?
Ru1 P1 2.3760(11) . ?
P1 C8 1.835(4) . ?
P1 C14 1.846(4) . ?
P1 B1 1.965(5) . ?
O1 C6 1.150(5) . ?
O2 C7 1.139(5) . ?
C1 C5 1.398(8) . ?
C1 C2 1.410(9) . ?
C2 C3 1.396(8) . ?
C3 C4 1.411(8) . ?
C4 C5 1.396(7) . ?
C8 C9 1.393(6) . ?
C8 C13 1.394(6) . ?
C9 C10 1.395(6) . ?
C10 C11 1.379(7) . ?
C11 C12 1.383(7) . ?
C12 C13 1.394(6) . ?
C14 C15 1.394(6) . ?
C14 C19 1.396(6) . ?
C15 C16 1.367(6) . ?
C16 C17 1.376(7) . ?
C17 C18 1.385(7) . ?
C18 C19 1.381(6) . ?
