#------------------------------------------------------------------------------
#$Date: 2017-01-05 00:36:38 +0200 (Thu, 05 Jan 2017) $
#$Revision: 189848 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/77/4317785.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_4317785
loop_
_publ_author_name
'Federico Roncaroli'
'Luis M. Baraldo'
'Leonardo D. Slep'
'José A. Olabe'
_publ_section_title
;
 Metallonitrosyl Fragment as Electron Acceptor: Intramolecular Charge
 Transfer, Long Range Electronic Coupling, and Electrophilic Reactivity in
 the trans-[NCRu(py)4(CN)Ru(py)4NO]3+ Ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1930
_journal_page_last               1939
_journal_paper_doi               10.1021/ic0109896
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C21 H24 Mo2 N2 O8'
_chemical_formula_weight         624.30
_chemical_name_common            compound2
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           shelxl
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8158(5)
_cell_length_b                   20.7844(11)
_cell_length_c                   11.7808(6)
_cell_measurement_temperature    298(2)
_cell_volume                     2383.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_method       'phi and omega 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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11776
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.8410
_exptl_absorpt_correction_T_min  0.6823
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       IRREGULAR
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.153
_refine_ls_goodness_of_fit_obs   1.157
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_restrained_S_obs      1.157
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_obs          0.0265
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0342P)²+1.3641P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0694
_refine_ls_wR_factor_obs         0.0682
_reflns_number_observed          4024
_reflns_number_total             4180
_reflns_observed_criterion       >2sigma(i)
_cod_data_source_file            ic0109896t_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
 Changing the capitalization of _atom_type_symbol data item
 values and the values of related data items (e. g. _atom_site_type_symbol).
 Updating the _chemical_formula_sum data item value.

 Antanas Vaitkus,
 2017-01-05

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+1.3641P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+1.3641P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'c21 h24 mo2 n2 o8'
_cod_database_code               4317785
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.31361(2) 0.583271(10) 0.72246(2) 0.03213(8) Uani 1 d . .
Mo2 Mo 0.14975(2) 0.628208(10) 0.78818(2) 0.03227(8) Uani 1 d . .
O1 O 0.5280(2) 0.58240(11) 0.6027(2) 0.0522(5) Uani 1 d . .
O2 O -0.0886(2) 0.69128(10) 0.7717(2) 0.0567(6) Uani 1 d . .
O3 O 0.3483(2) 0.52045(9) 0.8671(2) 0.0403(4) Uani 1 d . .
O4 O 0.1731(2) 0.56787(9) 0.9354(2) 0.0418(4) Uani 1 d . .
O5 O 0.1861(2) 0.50965(9) 0.6449(2) 0.0413(4) Uani 1 d . .
O6 O 0.0100(2) 0.55777(10) 0.7117(2) 0.0426(4) Uani 1 d . .
O7 O 0.4571(2) 0.64573(9) 0.8194(2) 0.0411(4) Uani 1 d . .
O8 O 0.2817(2) 0.69183(9) 0.8903(2) 0.0396(4) Uani 1 d . .
N1 N 0.2870(2) 0.64161(11) 0.5711(2) 0.0343(5) Uani 1 d . .
N2 N 0.1193(2) 0.69557(11) 0.6503(2) 0.0346(5) Uani 1 d . .
C1 C 0.1950(3) 0.68847(13) 0.5653(2) 0.0350(6) Uani 1 d . .
C2 C 0.2701(3) 0.52738(13) 0.9442(2) 0.0398(6) Uani 1 d . .
C3 C 0.2953(4) 0.4874(2) 1.0505(3) 0.0568(8) Uani 1 d . .
C4 C 0.0607(3) 0.51096(14) 0.6625(2) 0.0430(6) Uani 1 d . .
C5 C -0.0300(4) 0.4555(2) 0.6235(4) 0.0596(9) Uani 1 d . .
C6 C 0.4099(3) 0.68369(13) 0.8898(2) 0.0407(6) Uani 1 d . .
C7 C 0.5079(4) 0.7191(2) 0.9753(4) 0.0581(9) Uani 1 d . .
C11 C 0.3562(3) 0.63073(12) 0.4738(2) 0.0351(6) Uani 1 d . .
C12 C 0.3041(3) 0.64735(15) 0.3624(3) 0.0423(6) Uani 1 d . .
C13 C 0.3791(4) 0.6362(2) 0.2718(3) 0.0530(8) Uani 1 d . .
C14 C 0.5057(4) 0.6073(2) 0.2917(3) 0.0580(9) Uani 1 d . .
C15 C 0.5593(3) 0.5892(2) 0.4012(3) 0.0498(8) Uani 1 d . .
C16 C 0.4848(3) 0.60017(14) 0.4917(2) 0.0400(6) Uani 1 d . .
C17 C 0.6614(4) 0.5552(3) 0.6285(4) 0.0673(10) Uani 1 d . .
C21 C 0.0344(2) 0.75118(12) 0.6506(2) 0.0336(5) Uani 1 d . .
C22 C 0.0569(3) 0.80855(14) 0.5964(2) 0.0393(6) Uani 1 d . .
C23 C -0.0296(3) 0.8608(2) 0.6020(3) 0.0484(7) Uani 1 d . .
C24 C -0.1396(3) 0.8564(2) 0.6630(3) 0.0511(8) Uani 1 d . .
C25 C -0.1633(3) 0.8005(2) 0.7199(3) 0.0479(7) Uani 1 d . .
C26 C -0.0763(3) 0.74821(13) 0.7152(2) 0.0396(6) Uani 1 d . .
C27 C -0.2039(4) 0.6833(2) 0.8317(5) 0.0712(12) Uani 1 d . .
H1 H 0.1842(27) 0.7166(13) 0.5019(23) 0.029(7) Uiso 1 d . .
H3A H 0.2137(54) 0.4846(22) 1.0842(40) 0.098(16) Uiso 1 d . .
H3B H 0.3697(60) 0.5037(26) 1.0979(47) 0.118(19) Uiso 1 d . .
H3C H 0.3192(61) 0.4513(30) 1.0363(49) 0.128(23) Uiso 1 d . .
H5A H -0.1027(53) 0.4692(23) 0.5727(43) 0.099(16) Uiso 1 d . .
H5B H 0.0138(54) 0.4297(26) 0.5853(44) 0.101(18) Uiso 1 d . .
H5C H -0.0571(50) 0.4333(23) 0.6760(42) 0.090(16) Uiso 1 d . .
H7A H 0.4726(36) 0.7348(17) 1.0375(31) 0.057(10) Uiso 1 d . .
H7B H 0.5789(49) 0.6919(22) 1.0018(38) 0.088(14) Uiso 1 d . .
H7C H 0.5390(45) 0.7516(22) 0.9303(38) 0.086(14) Uiso 1 d . .
H12 H 0.2256(36) 0.6646(16) 0.3476(27) 0.051(9) Uiso 1 d . .
H13 H 0.3428(36) 0.6462(17) 0.2017(31) 0.057(10) Uiso 1 d . .
H14 H 0.5489(40) 0.5963(18) 0.2357(33) 0.069(11) Uiso 1 d . .
H15 H 0.6356(40) 0.5725(17) 0.4162(31) 0.060(11) Uiso 1 d . .
H17A H 0.6731(47) 0.5181(23) 0.5917(39) 0.087(15) Uiso 1 d . .
H17B H 0.6828(45) 0.5497(21) 0.7081(42) 0.088(14) Uiso 1 d . .
H17C H 0.7282(45) 0.5852(20) 0.6127(35) 0.071(13) Uiso 1 d . .
H22 H 0.1253(32) 0.8134(14) 0.5595(25) 0.038(8) Uiso 1 d . .
H23 H -0.0103(39) 0.8987(19) 0.5712(31) 0.065(11) Uiso 1 d . .
H24 H -0.1880(38) 0.8884(18) 0.6726(30) 0.057(10) Uiso 1 d . .
H25 H -0.2364(32) 0.7968(14) 0.7630(25) 0.040(7) Uiso 1 d . .
H27A H -0.2803(52) 0.6818(22) 0.7746(40) 0.094(16) Uiso 1 d . .
H27B H -0.1939(42) 0.7157(21) 0.8984(37) 0.079(13) Uiso 1 d . .
H27C H -0.1941(43) 0.6453(22) 0.8674(38) 0.081(13) Uiso 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'
Mo Mo -1.6832 0.6857 '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'
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
Mo2 Mo1 O5 92.43(5) . . ?
Mo2 Mo1 O7 90.92(5) . . ?
O5 Mo1 O7 170.61(8) . . ?
Mo2 Mo1 O3 91.61(5) . . ?
O5 Mo1 O3 85.77(8) . . ?
O7 Mo1 O3 85.36(8) . . ?
Mo2 Mo1 N1 92.22(6) . . ?
O5 Mo1 N1 92.79(8) . . ?
O7 Mo1 N1 95.85(8) . . ?
O3 Mo1 N1 175.96(7) . . ?
Mo1 Mo2 O8 92.64(5) . . ?
Mo1 Mo2 O6 91.19(5) . . ?
O8 Mo2 O6 170.50(7) . . ?
Mo1 Mo2 O4 91.83(5) . . ?
O8 Mo2 O4 84.93(8) . . ?
O6 Mo2 O4 86.26(8) . . ?
Mo1 Mo2 N2 92.85(5) . . ?
O8 Mo2 N2 92.16(8) . . ?
O6 Mo2 N2 96.34(8) . . ?
O4 Mo2 N2 174.60(8) . . ?
C16 O1 C17 118.2(3) . . ?
C26 O2 C27 118.0(3) . . ?
C2 O3 Mo1 116.9(2) . . ?
C2 O4 Mo2 117.3(2) . . ?
C4 O5 Mo1 116.5(2) . . ?
C4 O6 Mo2 116.9(2) . . ?
C6 O7 Mo1 117.0(2) . . ?
C6 O8 Mo2 116.6(2) . . ?
C1 N1 C11 118.0(2) . . ?
C1 N1 Mo1 117.9(2) . . ?
C11 N1 Mo1 124.1(2) . . ?
C1 N2 C21 118.4(2) . . ?
C1 N2 Mo2 117.6(2) . . ?
C21 N2 Mo2 123.7(2) . . ?
N1 C1 N2 119.1(2) . . ?
O4 C2 O3 122.3(2) . . ?
O4 C2 C3 118.6(3) . . ?
O3 C2 C3 119.0(3) . . ?
O6 C4 O5 122.4(3) . . ?
O6 C4 C5 118.7(3) . . ?
O5 C4 C5 118.9(3) . . ?
O8 C6 O7 122.0(3) . . ?
O8 C6 C7 118.9(3) . . ?
O7 C6 C7 119.1(3) . . ?
C12 C11 C16 117.9(3) . . ?
C12 C11 N1 124.4(2) . . ?
C16 C11 N1 117.6(2) . . ?
C11 C12 C13 121.1(3) . . ?
C14 C13 C12 119.9(3) . . ?
C13 C14 C15 120.4(3) . . ?
C14 C15 C16 119.9(3) . . ?
O1 C16 C15 124.0(3) . . ?
O1 C16 C11 115.2(2) . . ?
C15 C16 C11 120.8(3) . . ?
C22 C21 C26 117.9(2) . . ?
C22 C21 N2 124.7(2) . . ?
C26 C21 N2 117.3(2) . . ?
C21 C22 C23 121.3(3) . . ?
C24 C23 C22 119.9(3) . . ?
C23 C24 C25 120.3(3) . . ?
C24 C25 C26 119.9(3) . . ?
O2 C26 C25 124.3(2) . . ?
O2 C26 C21 115.1(2) . . ?
C25 C26 C21 120.6(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
Mo1 Mo2 2.0933(3) . ?
Mo1 O5 2.109(2) . ?
Mo1 O7 2.135(2) . ?
Mo1 O3 2.139(2) . ?
Mo1 N1 2.144(2) . ?
Mo2 O8 2.114(2) . ?
Mo2 O6 2.125(2) . ?
Mo2 O4 2.129(2) . ?
Mo2 N2 2.136(2) . ?
O1 C16 1.372(4) . ?
O1 C17 1.422(4) . ?
O2 C26 1.371(3) . ?
O2 C27 1.419(4) . ?
O3 C2 1.271(3) . ?
O4 C2 1.265(3) . ?
O5 C4 1.275(3) . ?
O6 C4 1.267(4) . ?
O7 C6 1.274(3) . ?
O8 C6 1.270(3) . ?
N1 C1 1.324(3) . ?
N1 C11 1.425(3) . ?
N2 C1 1.330(3) . ?
N2 C21 1.425(3) . ?
C2 C3 1.496(4) . ?
C4 C5 1.493(5) . ?
C6 C7 1.493(4) . ?
C11 C12 1.388(4) . ?
C11 C16 1.405(4) . ?
C12 C13 1.392(4) . ?
C13 C14 1.373(5) . ?
C14 C15 1.380(5) . ?
C15 C16 1.388(4) . ?
C21 C22 1.384(4) . ?
C21 C26 1.406(4) . ?
C22 C23 1.386(4) . ?
C23 C24 1.375(5) . ?
C24 C25 1.376(5) . ?
C25 C26 1.388(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Mo1 Mo2 N2 -4.46(8) . . . . ?
N1 Mo1 Mo2 O4 178.24(8) . . . . ?
N1 Mo1 Mo2 O6 91.95(8) . . . . ?
N1 Mo1 Mo2 O8 -96.75(8) . . . . ?
O3 Mo1 Mo2 N2 176.82(8) . . . . ?
O3 Mo1 Mo2 O4 -0.48(7) . . . . ?
O3 Mo1 Mo2 O6 -86.78(8) . . . . ?
O3 Mo1 Mo2 O8 84.53(7) . . . . ?
O5 Mo1 Mo2 N2 -97.34(8) . . . . ?
O5 Mo1 Mo2 O4 85.36(8) . . . . ?
O5 Mo1 Mo2 O6 -0.94(7) . . . . ?
O5 Mo1 Mo2 O8 170.36(7) . . . . ?
O7 Mo1 Mo2 N2 91.43(8) . . . . ?
O7 Mo1 Mo2 O4 -85.87(8) . . . . ?
O7 Mo1 Mo2 O6 -172.16(7) . . . . ?
O7 Mo1 Mo2 O8 -0.86(7) . . . . ?
