#------------------------------------------------------------------------------
#$Date: 2017-10-24 01:44:03 +0300 (Tue, 24 Oct 2017) $
#$Revision: 202252 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/66/4126626.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_4126626
loop_
_publ_author_name
'Shaffer, David W.'
'Xie, Yan'
'Szalda, David J.'
'Concepcion, Javier J.'
_publ_section_title
;
 Lability and Basicity of Bipyridine-Carboxylate-Phosphonate Ligand
 Accelerate Single-Site Water Oxidation by Ruthenium-Based Molecular
 Catalysts.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b06096
_journal_year                    2017
_chemical_formula_sum            'C29 H32 N4 O11 P Ru'
_chemical_formula_weight         744.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.283(3)
_cell_angle_beta                 104.321(3)
_cell_angle_gamma                116.898(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0051(5)
_cell_length_b                   12.0135(5)
_cell_length_c                   13.5167(6)
_cell_measurement_reflns_used    4597
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.93
_cell_measurement_theta_min      2.67
_cell_volume                     1525.42(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.1049
_diffrn_reflns_av_sigmaI/netI    0.1092
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52545
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
      SADABS Version 2007/2 (Sheldrick, Bruker AXS Inc.) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0570
_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)+(0.0504P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                5614
_reflns_number_total             8806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b06096_si_003.cif
_cod_data_source_block           ds0506
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4126626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.76834(3) 0.85108(3) 0.65209(2) 0.02210(9) Uani 1 1 d .
P1 P 0.87919(10) 1.11751(9) 0.76816(8) 0.0276(2) Uani 1 1 d .
O11 O 0.8112(2) 1.0331(2) 0.65964(18) 0.0282(6) Uani 1 1 d .
O12 O 0.8041(3) 1.1913(3) 0.7786(2) 0.0452(7) Uani 1 1 d .
O13 O 1.0374(3) 1.1882(3) 0.7972(2) 0.0459(8) Uani 1 1 d .
N11 N 0.7894(3) 0.8768(3) 0.8028(2) 0.0237(6) Uani 1 1 d .
C12 C 0.7561(3) 0.7727(3) 0.8519(3) 0.0261(8) Uani 1 1 d .
C13 C 0.7656(4) 0.7864(4) 0.9554(3) 0.0326(9) Uani 1 1 d .
H13 H 0.7444 0.7156 0.9909 0.039 Uiso 1 1 calc R
C14 C 0.8062(4) 0.9037(4) 1.0072(3) 0.0337(9) Uani 1 1 d .
H14 H 0.8100 0.9131 1.0780 0.040 Uiso 1 1 calc R
C15 C 0.8411(4) 1.0071(4) 0.9566(3) 0.0310(9) Uani 1 1 d .
H15 H 0.8708 1.0879 0.9929 0.037 Uiso 1 1 calc R
C16 C 0.8330(3) 0.9934(3) 0.8525(3) 0.0253(8) Uani 1 1 d .
N21 N 0.7167(3) 0.6787(3) 0.6848(2) 0.0251(7) Uani 1 1 d .
C22 C 0.7145(3) 0.6568(3) 0.7822(3) 0.0266(8) Uani 1 1 d .
C23 C 0.6796(4) 0.5365(3) 0.8053(3) 0.0338(9) Uani 1 1 d .
H23 H 0.6761 0.5186 0.8730 0.041 Uiso 1 1 calc R
C24 C 0.6498(4) 0.4429(4) 0.7283(3) 0.0424(11) Uani 1 1 d .
H24 H 0.6265 0.3601 0.7435 0.051 Uiso 1 1 calc R
C25 C 0.6533(4) 0.4677(4) 0.6287(3) 0.0361(9) Uani 1 1 d .
H25 H 0.6338 0.4031 0.5762 0.043 Uiso 1 1 calc R
C26 C 0.6857(3) 0.5877(3) 0.6082(3) 0.0262(8) Uani 1 1 d .
C27 C 0.6940(3) 0.6357(4) 0.5065(3) 0.0275(8) Uani 1 1 d .
O271 O 0.7362(3) 0.7566(2) 0.51110(18) 0.0288(6) Uani 1 1 d .
O272 O 0.6648(3) 0.5645(2) 0.4283(2) 0.0352(6) Uani 1 1 d .
N51 N 0.9847(3) 0.9043(3) 0.6868(2) 0.0238(6) Uani 1 1 d .
C52 C 1.0521(3) 0.8581(3) 0.7541(3) 0.0240(8) Uani 1 1 d .
H52 H 0.9982 0.7935 0.7883 0.029 Uiso 1 1 calc R
C53 C 1.1997(4) 0.8996(3) 0.7780(3) 0.0252(8) Uani 1 1 d .
C54 C 1.2783(3) 0.9919(3) 0.7244(3) 0.0264(8) Uani 1 1 d .
C55 C 1.2040(4) 1.0397(3) 0.6516(3) 0.0303(9) Uani 1 1 d .
H54 H 1.2533 1.1025 0.6142 0.036 Uiso 1 1 calc R
C56 C 1.0632(4) 0.9953(3) 0.6361(3) 0.0275(8) Uani 1 1 d .
H56 H 1.0157 1.0288 0.5873 0.033 Uiso 1 1 calc R
C57 C 1.2685(4) 0.8509(4) 0.8543(3) 0.0325(9) Uani 1 1 d .
H57 H 1.2153 0.7880 0.8899 0.039 Uiso 1 1 calc R
C58 C 1.4120(4) 0.8958(4) 0.8756(3) 0.0387(10) Uani 1 1 d .
H58 H 1.4589 0.8649 0.9276 0.046 Uiso 1 1 calc R
C59 C 1.4912(4) 0.9870(4) 0.8220(3) 0.0393(10) Uani 1 1 d .
H59 H 1.5907 1.0159 0.8372 0.047 Uiso 1 1 calc R
C50 C 1.4267(4) 1.0347(4) 0.7479(3) 0.0344(9) Uani 1 1 d .
H50 H 1.4815 1.0966 0.7123 0.041 Uiso 1 1 calc R
N61 N 0.5539(3) 0.8065(3) 0.6082(2) 0.0250(6) Uani 1 1 d .
C62 C 0.4571(4) 0.7353(3) 0.6526(3) 0.0282(8) Uani 1 1 d .
H62 H 0.4866 0.7020 0.7115 0.034 Uiso 1 1 calc R
C63 C 0.3121(4) 0.7055(3) 0.6176(3) 0.0301(8) Uani 1 1 d .
C64 C 0.2687(4) 0.7544(4) 0.5299(3) 0.0337(9) Uani 1 1 d .
C65 C 0.3731(4) 0.8298(4) 0.4823(3) 0.0345(9) Uani 1 1 d .
H65 H 0.3475 0.8635 0.4225 0.041 Uiso 1 1 calc R
C66 C 0.5100(4) 0.8537(3) 0.5225(3) 0.0289(8) Uani 1 1 d .
H66 H 0.5788 0.9055 0.4900 0.035 Uiso 1 1 calc R
C67 C 0.2124(4) 0.6281(4) 0.6679(3) 0.0413(10) Uani 1 1 d .
H67 H 0.2418 0.5945 0.7267 0.050 Uiso 1 1 calc R
C68 C 0.0732(4) 0.6021(4) 0.6309(4) 0.0492(12) Uani 1 1 d .
H68 H 0.0061 0.5516 0.6651 0.059 Uiso 1 1 calc R
C69 C 0.0292(4) 0.6491(4) 0.5436(4) 0.0515(13) Uani 1 1 d .
H69 H -0.0684 0.6279 0.5180 0.062 Uiso 1 1 calc R
C60 C 0.1228(4) 0.7248(4) 0.4939(4) 0.0452(11) Uani 1 1 d .
H60 H 0.0909 0.7577 0.4357 0.054 Uiso 1 1 calc R
OW1 O 0.2657(4) 0.7027(3) 0.0817(2) 0.0640(10) Uani 1 1 d .
H1A H 0.2379 0.7501 0.1207 0.077 Uiso 1 1 d .
H1B H 0.1961 0.6786 0.0312 0.077 Uiso 1 1 d .
OW2 O 0.7002(3) 0.6683(3) 0.2347(2) 0.0482(8) Uani 1 1 d .
H2A H 0.7946 0.7164 0.2144 0.058 Uiso 1 1 d .
H2B H 0.7182 0.6675 0.2993 0.058 Uiso 1 1 d .
OW3 O 0.5144(3) 0.7119(3) 0.0716(2) 0.0629(9) Uani 1 1 d .
H3A H 0.5550 0.6782 0.1270 0.076 Uiso 1 1 d .
H3B H 0.4791 0.6436 0.0398 0.076 Uiso 1 1 d .
OW4 O -0.0011(4) 0.6322(4) -0.0697(3) 0.0903(14) Uani 1 1 d .
H4A H -0.0190 0.5476 -0.1157 0.108 Uiso 1 1 d .
H4B H -0.0784 0.5810 -0.0418 0.108 Uiso 1 1 d .
OM5A O 1.0387(13) 1.4508(8) 0.8593(12) 0.142(6) Uani 0.50 1 d P
OM5B O 0.8672(11) 0.5692(8) 1.0961(7) 0.084(3) Uani 0.50 1 d P
OW6A O 0.6771(12) 0.4966(9) 0.0769(7) 0.097(3) Uani 0.50 1 d P
OW6B O 0.5959(9) 0.4291(7) 0.1202(7) 0.075(2) Uani 0.50 1 d P
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'
O O 0.0106 0.0060 '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
N21 Ru1 N11 78.62(12) . .
N21 Ru1 O11 162.93(11) . .
N11 Ru1 O11 84.94(11) . .
N21 Ru1 O271 78.96(11) . .
N11 Ru1 O271 157.39(11) . .
O11 Ru1 O271 117.63(10) . .
N21 Ru1 N51 93.54(11) . .
N11 Ru1 N51 89.36(11) . .
O11 Ru1 N51 90.83(10) . .
O271 Ru1 N51 89.12(10) . .
N21 Ru1 N61 90.11(11) . .
N11 Ru1 N61 93.91(11) . .
O11 Ru1 N61 86.40(10) . .
O271 Ru1 N61 89.04(11) . .
N51 Ru1 N61 175.51(11) . .
O12 P1 O13 116.99(18) . .
O12 P1 O11 110.37(16) . .
O13 P1 O11 113.09(15) . .
O12 P1 C16 108.16(16) . .
O13 P1 C16 106.45(16) . .
O11 P1 C16 100.21(15) . .
P1 O11 Ru1 118.46(13) . .
C16 N11 C12 122.5(3) . .
C16 N11 Ru1 120.0(2) . .
C12 N11 Ru1 117.5(2) . .
N11 C12 C13 119.0(4) . .
N11 C12 C22 112.6(3) . .
C13 C12 C22 128.4(3) . .
C12 C13 C14 119.6(4) . .
C12 C13 H13 120.2 . .
C14 C13 H13 120.2 . .
C15 C14 C13 120.3(4) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C14 C15 C16 120.1(4) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
N11 C16 C15 118.5(3) . .
N11 C16 P1 113.0(3) . .
C15 C16 P1 128.5(3) . .
C26 N21 C22 122.8(3) . .
C26 N21 Ru1 118.1(2) . .
C22 N21 Ru1 119.1(2) . .
N21 C22 C23 119.1(4) . .
N21 C22 C12 112.2(3) . .
C23 C22 C12 128.7(3) . .
C24 C23 C22 118.7(4) . .
C24 C23 H23 120.6 . .
C22 C23 H23 120.6 . .
C23 C24 C25 121.1(4) . .
C23 C24 H24 119.4 . .
C25 C24 H24 119.4 . .
C26 C25 C24 118.5(4) . .
C26 C25 H25 120.8 . .
C24 C25 H25 120.8 . .
N21 C26 C25 119.7(3) . .
N21 C26 C27 112.6(3) . .
C25 C26 C27 127.7(4) . .
O272 C27 O271 124.6(3) . .
O272 C27 C26 121.0(3) . .
O271 C27 C26 114.4(3) . .
C27 O271 Ru1 115.9(2) . .
C52 N51 C56 117.5(3) . .
C52 N51 Ru1 125.2(2) . .
C56 N51 Ru1 117.2(2) . .
N51 C52 C53 123.6(3) . .
N51 C52 H52 118.2 . .
C53 C52 H52 118.2 . .
C54 C53 C52 118.0(3) . .
C54 C53 C57 120.4(3) . .
C52 C53 C57 121.5(3) . .
C53 C54 C50 118.6(3) . .
C53 C54 C55 117.6(3) . .
C50 C54 C55 123.7(3) . .
C56 C55 C54 119.5(3) . .
C56 C55 H54 120.2 . .
C54 C55 H54 120.2 . .
C55 C56 N51 123.7(3) . .
C55 C56 H56 118.2 . .
N51 C56 H56 118.2 . .
C58 C57 C53 119.2(4) . .
C58 C57 H57 120.4 . .
C53 C57 H57 120.4 . .
C57 C58 C59 120.9(4) . .
C57 C58 H58 119.5 . .
C59 C58 H58 119.5 . .
C50 C59 C58 120.7(4) . .
C50 C59 H59 119.6 . .
C58 C59 H59 119.6 . .
C59 C50 C54 120.1(4) . .
C59 C50 H50 119.9 . .
C54 C50 H50 119.9 . .
C62 N61 C66 117.6(3) . .
C62 N61 Ru1 126.4(2) . .
C66 N61 Ru1 116.0(2) . .
N61 C62 C63 123.9(3) . .
N61 C62 H62 118.1 . .
C63 C62 H62 118.1 . .
C64 C63 C62 117.9(3) . .
C64 C63 C67 120.6(3) . .
C62 C63 C67 121.6(4) . .
C63 C64 C65 117.8(3) . .
C63 C64 C60 118.3(4) . .
C65 C64 C60 123.9(4) . .
C66 C65 C64 119.7(4) . .
C66 C65 H65 120.1 . .
C64 C65 H65 120.1 . .
C65 C66 N61 123.1(4) . .
C65 C66 H66 118.5 . .
N61 C66 H66 118.5 . .
C68 C67 C63 119.2(4) . .
C68 C67 H67 120.4 . .
C63 C67 H67 120.4 . .
C67 C68 C69 120.5(4) . .
C67 C68 H68 119.7 . .
C69 C68 H68 119.7 . .
C60 C69 C68 121.6(4) . .
C60 C69 H69 119.2 . .
C68 C69 H69 119.2 . .
C69 C60 C64 119.7(4) . .
C69 C60 H60 120.1 . .
C64 C60 H60 120.1 . .
H1A OW1 H1B 95.4(3) . .
H2A OW2 H2B 110.4(3) . .
H3A OW3 H3B 85.5(3) . .
H4A OW4 H4B 90.0(3) . .
OM5A OM5B OW6A 135.8(10) 2_777 1_556
OW6B OW6A OM5B 136.2(9) . 1_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N21 1.977(3) .
Ru1 N11 1.993(3) .
Ru1 O11 2.012(2) .
Ru1 O271 2.062(2) .
Ru1 N51 2.087(3) .
Ru1 N61 2.087(3) .
P1 O12 1.485(3) .
P1 O13 1.488(3) .
P1 O11 1.563(3) .
P1 C16 1.860(4) .
N11 C16 1.354(4) .
N11 C12 1.372(4) .
C12 C13 1.377(5) .
C12 C22 1.478(5) .
C13 C14 1.381(5) .
C13 H13 0.9500 .
C14 C15 1.376(5) .
C14 H14 0.9500 .
C15 C16 1.389(5) .
C15 H15 0.9500 .
N21 C26 1.349(4) .
N21 C22 1.353(4) .
C22 C23 1.383(5) .
C23 C24 1.378(6) .
C23 H23 0.9500 .
C24 C25 1.391(6) .
C24 H24 0.9500 .
C25 C26 1.373(5) .
C25 H25 0.9500 .
C26 C27 1.510(5) .
C27 O272 1.222(4) .
C27 O271 1.304(4) .
N51 C52 1.323(4) .
N51 C56 1.372(4) .
C52 C53 1.411(5) .
C52 H52 0.9500 .
C53 C54 1.408(5) .
C53 C57 1.420(5) .
C54 C50 1.418(5) .
C54 C55 1.420(5) .
C55 C56 1.348(5) .
C55 H54 0.9500 .
C56 H56 0.9500 .
C57 C58 1.366(5) .
C57 H57 0.9500 .
C58 C59 1.403(6) .
C58 H58 0.9500 .
C59 C50 1.371(5) .
C59 H59 0.9500 .
C50 H50 0.9500 .
N61 C62 1.319(4) .
N61 C66 1.377(4) .
C62 C63 1.415(5) .
C62 H62 0.9500 .
C63 C64 1.409(5) .
C63 C67 1.416(5) .
C64 C65 1.415(6) .
C64 C60 1.425(5) .
C65 C66 1.358(5) .
C65 H65 0.9500 .
C66 H66 0.9500 .
C67 C68 1.370(5) .
C67 H67 0.9500 .
C68 C69 1.394(7) .
C68 H68 0.9500 .
C69 C60 1.364(6) .
C69 H69 0.9500 .
C60 H60 0.9500 .
OW1 H1A 0.959(3) .
OW1 H1B 0.817(3) .
OW2 H2A 1.045(3) .
OW2 H2B 0.848(3) .
OW3 H3A 0.967(3) .
OW3 H3B 0.789(4) .
OW4 H4A 1.090(5) .
OW4 H4B 0.970(4) .
OM5A OM5B 1.189(15) 2_777
OM5B OM5A 1.189(15) 2_777
OM5B OW6A 1.809(14) 1_556
OW6A OW6B 1.192(11) .
OW6A OM5B 1.809(14) 1_554
