#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:16:34 +0100 (vie 25 de mar de 2016) $
#$Revision: 179746 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/42/7004231.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_7004231
loop_
_publ_author_name
'Gott, Andrew L.'
'McGowan, Patrick C.'
'Podesta, Thomas J.'
_publ_section_title
;
 Controlling the binding of dihydrogen using ruthenium complexes
 containing N-mono-functionalised 1,4,7-triazacyclononane ligand
 systems
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              3729
_journal_page_last               3738
_journal_paper_doi               10.1039/b804572k
_journal_year                    2008
_chemical_formula_sum            'C34 H41 B2 F8 N4 O2 P Ru'
_chemical_formula_weight         843.37
_chemical_name_common            'in paper 5'
_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                 95.0030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3690(2)
_cell_length_b                   12.4991(2)
_cell_length_c                   23.0691(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3552.93(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36076
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.8951
_exptl_absorpt_correction_T_min  0.8951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0307
_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)+(0.0303P)²+2.6835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                5993
_reflns_number_total             6976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804572k.txt
_cod_data_source_block           alg5
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7004231
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 -0.190264(14) 0.177225(13) 0.088525(7) 0.01869(7) Uani 1 1 d . . .
C1 C -0.10728(19) 0.21090(17) 0.02824(10) 0.0233(5) Uani 1 1 d . . .
O1 O -0.05587(14) 0.22645(14) -0.01035(7) 0.0330(4) Uani 1 1 d . . .
N1 N -0.07885(16) 0.06191(14) 0.12592(8) 0.0231(4) Uani 1 1 d . . .
C2 C -0.0716(2) -0.02087(18) 0.07942(10) 0.0261(5) Uani 1 1 d . . .
H2A H -0.0312 -0.0840 0.0957 0.031 Uiso 1 1 calc R . .
H2B H -0.0321 0.0087 0.0475 0.031 Uiso 1 1 calc R . .
C3 C -0.1856(2) -0.05400(17) 0.05598(10) 0.0269(5) Uani 1 1 d . . .
H3A H -0.1818 -0.0931 0.0189 0.032 Uiso 1 1 calc R . .
H3B H -0.2159 -0.1032 0.0840 0.032 Uiso 1 1 calc R . .
N4 N -0.26058(15) 0.04161(14) 0.04576(8) 0.0226(4) Uani 1 1 d . . .
H4 H -0.2705 0.0554 0.0060 0.027 Uiso 1 1 calc R . .
C5 C -0.36821(19) 0.02328(18) 0.06805(10) 0.0256(5) Uani 1 1 d . . .
H5A H -0.3969 -0.0472 0.0546 0.031 Uiso 1 1 calc R . .
H5B H -0.4198 0.0790 0.0526 0.031 Uiso 1 1 calc R . .
C6 C -0.35776(19) 0.02668(18) 0.13422(10) 0.0261(5) Uani 1 1 d . . .
H6A H -0.4304 0.0368 0.1483 0.031 Uiso 1 1 calc R . .
H6B H -0.3284 -0.0424 0.1496 0.031 Uiso 1 1 calc R . .
N7 N -0.28378(15) 0.11645(15) 0.15673(8) 0.0232(4) Uani 1 1 d . . .
H7 H -0.3254 0.1716 0.1702 0.028 Uiso 1 1 calc R . .
C8 C -0.20334(19) 0.08004(19) 0.20498(10) 0.0261(5) Uani 1 1 d . . .
H8A H -0.2407 0.0377 0.2335 0.031 Uiso 1 1 calc R . .
H8B H -0.1692 0.1429 0.2253 0.031 Uiso 1 1 calc R . .
C9 C -0.1172(2) 0.01221(18) 0.17999(10) 0.0257(5) Uani 1 1 d . . .
H9A H -0.0547 0.0037 0.2095 0.031 Uiso 1 1 calc R . .
H9B H -0.1471 -0.0598 0.1705 0.031 Uiso 1 1 calc R . .
C10 C 0.02384(19) 0.12264(18) 0.13927(11) 0.0268(5) Uani 1 1 d . . .
H10A H 0.0590 0.1354 0.1030 0.032 Uiso 1 1 calc R . .
H10B H 0.0743 0.0804 0.1660 0.032 Uiso 1 1 calc R . .
C11 C -0.00012(19) 0.22784(19) 0.16711(10) 0.0255(5) Uani 1 1 d . . .
N12 N -0.09834(15) 0.27304(15) 0.14997(8) 0.0219(4) Uani 1 1 d . . .
C13 C -0.1243(2) 0.36607(18) 0.17498(10) 0.0253(5) Uani 1 1 d . . .
H13 H -0.1941 0.3959 0.1650 0.030 Uiso 1 1 calc R . .
C14 C -0.0533(2) 0.4197(2) 0.21451(10) 0.0302(5) Uani 1 1 d . . .
H14 H -0.0736 0.4858 0.2307 0.036 Uiso 1 1 calc R . .
C15 C 0.0478(2) 0.3758(2) 0.23010(11) 0.0346(6) Uani 1 1 d . . .
H15 H 0.0986 0.4123 0.2563 0.041 Uiso 1 1 calc R . .
C16 C 0.0736(2) 0.2778(2) 0.20695(11) 0.0329(6) Uani 1 1 d . . .
H16 H 0.1415 0.2450 0.2183 0.039 Uiso 1 1 calc R . .
P1 P -0.31547(5) 0.30503(4) 0.05008(2) 0.01982(13) Uani 1 1 d . . .
C111 C -0.25730(18) 0.42797(17) 0.02188(9) 0.0219(5) Uani 1 1 d . . .
C112 C -0.1541(2) 0.46296(19) 0.04211(10) 0.0275(5) Uani 1 1 d . . .
H112 H -0.1109 0.4208 0.0695 0.033 Uiso 1 1 calc R . .
C113 C -0.1134(2) 0.55899(19) 0.02264(11) 0.0335(6) Uani 1 1 d . . .
H113 H -0.0438 0.5832 0.0378 0.040 Uiso 1 1 calc R . .
C114 C -0.1740(2) 0.61940(19) -0.01871(11) 0.0303(5) Uani 1 1 d . . .
H114 H -0.1464 0.6850 -0.0320 0.036 Uiso 1 1 calc R . .
C115 C -0.2749(2) 0.58338(19) -0.04041(11) 0.0299(5) Uani 1 1 d . . .
H115 H -0.3157 0.6235 -0.0697 0.036 Uiso 1 1 calc R . .
C116 C -0.3175(2) 0.48938(19) -0.02013(10) 0.0272(5) Uani 1 1 d . . .
H116 H -0.3879 0.4665 -0.0348 0.033 Uiso 1 1 calc R . .
C121 C -0.40903(18) 0.35256(18) 0.10141(9) 0.0218(5) Uani 1 1 d . . .
C122 C -0.40815(19) 0.45821(18) 0.12068(10) 0.0259(5) Uani 1 1 d . . .
H122 H -0.3588 0.5080 0.1064 0.031 Uiso 1 1 calc R . .
C123 C -0.4792(2) 0.49119(19) 0.16077(10) 0.0305(5) Uani 1 1 d . . .
H123 H -0.4783 0.5635 0.1735 0.037 Uiso 1 1 calc R . .
C124 C -0.5513(2) 0.4196(2) 0.18230(10) 0.0298(5) Uani 1 1 d . . .
H124 H -0.5998 0.4428 0.2094 0.036 Uiso 1 1 calc R . .
C125 C -0.5522(2) 0.31379(19) 0.16404(10) 0.0277(5) Uani 1 1 d . . .
H125 H -0.6006 0.2641 0.1791 0.033 Uiso 1 1 calc R . .
C126 C -0.48208(18) 0.28066(18) 0.12357(10) 0.0242(5) Uani 1 1 d . . .
H126 H -0.4837 0.2084 0.1108 0.029 Uiso 1 1 calc R . .
C131 C -0.40299(19) 0.26337(17) -0.01404(10) 0.0225(5) Uani 1 1 d . . .
C132 C -0.3536(2) 0.22113(18) -0.06113(10) 0.0274(5) Uani 1 1 d . . .
H132 H -0.2782 0.2050 -0.0572 0.033 Uiso 1 1 calc R . .
C133 C -0.4139(2) 0.2026(2) -0.11356(10) 0.0322(6) Uani 1 1 d . . .
H133 H -0.3797 0.1734 -0.1453 0.039 Uiso 1 1 calc R . .
C134 C -0.5233(2) 0.22616(19) -0.12013(10) 0.0313(6) Uani 1 1 d . . .
H134 H -0.5637 0.2152 -0.1566 0.038 Uiso 1 1 calc R . .
C135 C -0.5741(2) 0.26587(19) -0.07332(11) 0.0301(5) Uani 1 1 d . . .
H135 H -0.6497 0.2806 -0.0775 0.036 Uiso 1 1 calc R . .
C136 C -0.51435(19) 0.28407(18) -0.02035(10) 0.0264(5) Uani 1 1 d . . .
H136 H -0.5495 0.3107 0.0117 0.032 Uiso 1 1 calc R . .
B1 B -0.2953(2) -0.0664(2) -0.09940(13) 0.0326(6) Uani 1 1 d . . .
F11 F -0.37643(13) -0.06126(15) -0.06148(8) 0.0530(5) Uani 1 1 d . . .
F12 F -0.33802(18) -0.04262(15) -0.15480(7) 0.0668(6) Uani 1 1 d . . .
F13 F -0.24967(13) -0.16729(11) -0.09789(8) 0.0459(4) Uani 1 1 d . . .
F14 F -0.21496(12) 0.00869(11) -0.08050(7) 0.0386(4) Uani 1 1 d . . .
B2 B -0.1706(2) -0.2897(2) 0.18887(12) 0.0289(6) Uani 1 1 d . . .
F21 F -0.11176(13) -0.24518(12) 0.14647(7) 0.0407(4) Uani 1 1 d . . .
F22 F -0.10137(12) -0.31890(12) 0.23712(6) 0.0376(4) Uani 1 1 d . . .
F23 F -0.24502(13) -0.21463(13) 0.20595(8) 0.0494(4) Uani 1 1 d . . .
F24 F -0.22554(14) -0.38013(12) 0.16729(6) 0.0429(4) Uani 1 1 d . . .
O1S O 0.2393(2) 0.1229(2) 0.28377(11) 0.0698(7) Uani 1 1 d . . .
C1S C 0.3111(2) 0.1620(3) 0.31721(13) 0.0477(8) Uani 1 1 d . . .
C2S C 0.3444(3) 0.2758(3) 0.31367(15) 0.0549(8) Uani 1 1 d . . .
H2S1 H 0.2966 0.3125 0.2839 0.082 Uiso 1 1 calc R . .
H2S2 H 0.4195 0.2796 0.3034 0.082 Uiso 1 1 calc R . .
H2S3 H 0.3390 0.3104 0.3514 0.082 Uiso 1 1 calc R . .
C3S C 0.3696(3) 0.0964(3) 0.36365(13) 0.0558(9) Uani 1 1 d . . .
H3S1 H 0.3477 0.0214 0.3588 0.084 Uiso 1 1 calc R . .
H3S2 H 0.3517 0.1220 0.4018 0.084 Uiso 1 1 calc R . .
H3S3 H 0.4480 0.1026 0.3610 0.084 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'
O O 0.0106 0.0060 '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'
F F 0.0171 0.0103 '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
C1 Ru1 N4 93.69(9) . . ?
C1 Ru1 N12 94.26(8) . . ?
N4 Ru1 N12 161.02(7) . . ?
C1 Ru1 N1 94.41(9) . . ?
N4 Ru1 N1 82.60(7) . . ?
N12 Ru1 N1 79.62(7) . . ?
C1 Ru1 N7 172.67(8) . . ?
N4 Ru1 N7 80.43(7) . . ?
N12 Ru1 N7 90.09(7) . . ?
N1 Ru1 N7 80.56(7) . . ?
C1 Ru1 P1 87.25(7) . . ?
N4 Ru1 P1 97.97(5) . . ?
N12 Ru1 P1 99.60(5) . . ?
N1 Ru1 P1 178.20(5) . . ?
N7 Ru1 P1 97.85(5) . . ?
O1 C1 Ru1 176.4(2) . . ?
C10 N1 C2 113.38(18) . . ?
C10 N1 C9 111.31(17) . . ?
C2 N1 C9 110.53(17) . . ?
C10 N1 Ru1 104.46(13) . . ?
C2 N1 Ru1 104.76(13) . . ?
C9 N1 Ru1 112.09(14) . . ?
N1 C2 C3 109.31(19) . . ?
N4 C3 C2 112.03(18) . . ?
C5 N4 C3 112.23(17) . . ?
C5 N4 Ru1 107.89(13) . . ?
C3 N4 Ru1 109.77(13) . . ?
N4 C5 C6 110.04(18) . . ?
N7 C6 C5 111.20(18) . . ?
C8 N7 C6 111.90(17) . . ?
C8 N7 Ru1 106.48(14) . . ?
C6 N7 Ru1 110.84(13) . . ?
N7 C8 C9 109.34(18) . . ?
N1 C9 C8 111.53(18) . . ?
N1 C10 C11 109.74(19) . . ?
N12 C11 C16 121.5(2) . . ?
N12 C11 C10 116.2(2) . . ?
C16 C11 C10 122.3(2) . . ?
C13 N12 C11 118.12(19) . . ?
C13 N12 Ru1 129.93(15) . . ?
C11 N12 Ru1 111.89(15) . . ?
N12 C13 C14 122.6(2) . . ?
C13 C14 C15 119.1(2) . . ?
C14 C15 C16 119.0(2) . . ?
C15 C16 C11 119.6(2) . . ?
C121 P1 C131 104.65(10) . . ?
C121 P1 C111 104.31(10) . . ?
C131 P1 C111 100.01(10) . . ?
C121 P1 Ru1 114.30(7) . . ?
C131 P1 Ru1 115.87(7) . . ?
C111 P1 Ru1 115.92(7) . . ?
C112 C111 C116 118.5(2) . . ?
C112 C111 P1 121.32(17) . . ?
C116 C111 P1 120.16(17) . . ?
C111 C112 C113 120.7(2) . . ?
C114 C113 C112 120.2(2) . . ?
C115 C114 C113 119.4(2) . . ?
C114 C115 C116 120.9(2) . . ?
C115 C116 C111 120.3(2) . . ?
C122 C121 C126 118.6(2) . . ?
C122 C121 P1 121.85(18) . . ?
C126 C121 P1 119.54(17) . . ?
C123 C122 C121 120.3(2) . . ?
C124 C123 C122 120.7(2) . . ?
C123 C124 C125 119.7(2) . . ?
C124 C125 C126 119.9(2) . . ?
C125 C126 C121 120.9(2) . . ?
C132 C131 C136 118.9(2) . . ?
C132 C131 P1 117.91(18) . . ?
C136 C131 P1 122.68(18) . . ?
C133 C132 C131 120.3(2) . . ?
C134 C133 C132 120.6(2) . . ?
C133 C134 C135 119.8(2) . . ?
C134 C135 C136 120.0(2) . . ?
C135 C136 C131 120.3(2) . . ?
F12 B1 F13 110.2(2) . . ?
F12 B1 F11 109.6(2) . . ?
F13 B1 F11 110.0(2) . . ?
F12 B1 F14 110.4(2) . . ?
F13 B1 F14 109.0(2) . . ?
F11 B1 F14 107.7(2) . . ?
F21 B2 F24 110.2(2) . . ?
F21 B2 F22 110.2(2) . . ?
F24 B2 F22 108.7(2) . . ?
F21 B2 F23 109.2(2) . . ?
F24 B2 F23 109.5(2) . . ?
F22 B2 F23 109.0(2) . . ?
O1S C1S C2S 122.4(3) . . ?
O1S C1S C3S 120.9(3) . . ?
C2S C1S C3S 116.6(3) . . ?
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 C1 1.848(2) . ?
Ru1 N4 2.1103(18) . ?
Ru1 N12 2.1107(18) . ?
Ru1 N1 2.1244(18) . ?
Ru1 N7 2.1699(19) . ?
Ru1 P1 2.3445(6) . ?
C1 O1 1.155(3) . ?
N1 C10 1.489(3) . ?
N1 C2 1.499(3) . ?
N1 C9 1.507(3) . ?
C2 C3 1.523(3) . ?
C3 N4 1.519(3) . ?
N4 C5 1.486(3) . ?
C5 C6 1.521(3) . ?
C6 N7 1.511(3) . ?
N7 C8 1.498(3) . ?
C8 C9 1.515(3) . ?
C10 C11 1.504(3) . ?
C11 N12 1.367(3) . ?
C11 C16 1.386(3) . ?
N12 C13 1.349(3) . ?
C13 C14 1.383(3) . ?
C14 C15 1.384(4) . ?
C15 C16 1.385(4) . ?
P1 C121 1.826(2) . ?
P1 C131 1.831(2) . ?
P1 C111 1.840(2) . ?
C111 C112 1.391(3) . ?
C111 C116 1.399(3) . ?
C112 C113 1.391(3) . ?
C113 C114 1.385(3) . ?
C114 C115 1.379(3) . ?
C115 C116 1.386(3) . ?
C121 C122 1.393(3) . ?
C121 C126 1.402(3) . ?
C122 C123 1.393(3) . ?
C123 C124 1.385(4) . ?
C124 C125 1.388(3) . ?
C125 C126 1.391(3) . ?
C131 C132 1.396(3) . ?
C131 C136 1.397(3) . ?
C132 C133 1.384(3) . ?
C133 C134 1.380(4) . ?
C134 C135 1.388(4) . ?
C135 C136 1.391(3) . ?
B1 F12 1.372(3) . ?
B1 F13 1.381(3) . ?
B1 F11 1.389(3) . ?
B1 F14 1.408(3) . ?
B2 F21 1.386(3) . ?
B2 F24 1.388(3) . ?
B2 F22 1.392(3) . ?
B2 F23 1.395(3) . ?
O1S C1S 1.226(4) . ?
C1S C2S 1.485(5) . ?
C1S C3S 1.487(4) . ?
