#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:50:38 +0100 (jue 07 de nov de 2019) $
#$Revision: 223871 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/00/7700095.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_7700095
loop_
_publ_author_name
'Damjanović, Vladimir'
'Pisk, Jana'
'Kuzman, Dino'
'Agustin, Dominique'
'Vrdoljak, Višnja'
'Stilinović, Vladimir'
'Cindrić, Marina'
_publ_section_title
;
 The synthesis, structure and catalytic properties of the
 [Mo₇O₂₄(μ-Mo₈O₂₆)Mo₇O₂₄]¹⁶⁻
 anion formed via two intermediate heptamolybdates
 [Co(en)₃]₂[NaMo₇O₂₄]Cl·nH₂O
 and
 (H₃O)[Co(en)₃]₂[Mo₇O₂₄]Cl·9H₂O.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9974
_journal_page_last               9983
_journal_paper_doi               10.1039/c9dt01625b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C9 H19 Co N4 O8'
_chemical_formula_weight         370.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-03-21 deposited with the CCDC.    2019-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.534(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3394(3)
_cell_length_b                   12.0376(4)
_cell_length_c                   12.8993(4)
_cell_measurement_reflns_used    5529
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      37.3764
_cell_measurement_theta_min      3.7290
_cell_volume                     1447.43(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics
;
Mercury CSD 3.10.3 (Build 205818) 
Created on uto kol 14 05:36:29 2018
;
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9501
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.993
_diffrn_reflns_theta_min         3.956
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3148
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0323P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2471
_reflns_number_total             3148
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01625b2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7700094--7700099.cif.'
_cod_database_code               7700095
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Co1 Co 0.05692(2) 0.58085(2) 0.20066(2) 0.01842(7) Uani 1 1 d . .
O6 O 0.27809(19) 0.33752(15) 0.02515(12) 0.0625(5) Uani 1 1 d . .
O1 O -0.00951(13) 0.73134(9) 0.18404(8) 0.0246(3) Uani 1 1 d . .
O3 O 0.08560(16) 0.71033(10) -0.07371(8) 0.0355(3) Uani 1 1 d . .
O2 O 0.11107(13) 0.59444(9) 0.06031(8) 0.0238(3) Uani 1 1 d . .
O5 O 0.39238(18) 0.31416(14) -0.11766(11) 0.0502(4) Uani 1 1 d . .
N4 N -0.01054(17) 0.57443(14) 0.33880(11) 0.0244(3) Uani 1 1 d . .
O4 O -0.03945(16) 0.86030(10) 0.06064(9) 0.0358(3) Uani 1 1 d . .
N2 N 0.13814(17) 0.43228(12) 0.20691(12) 0.0231(3) Uani 1 1 d . .
O8 O 0.59961(17) 0.19548(13) -0.12167(11) 0.0476(4) Uani 1 1 d . .
N3 N -0.13078(17) 0.52421(13) 0.15393(11) 0.0244(3) Uani 1 1 d D .
C8 C 0.4768(3) 0.2149(3) 0.03247(18) 0.0818(11) Uani 1 1 d . .
H8A H 0.5201 0.2519 0.0934 0.098 Uiso 1 1 calc R U
H8B H 0.4204 0.1537 0.0572 0.098 Uiso 1 1 calc R U
O7 O 0.67826(19) 0.10110(15) 0.01899(12) 0.0609(5) Uani 1 1 d . .
C1 C 0.00021(19) 0.76856(13) 0.09078(12) 0.0242(4) Uani 1 1 d . .
C4 C 0.2801(2) 0.43455(16) 0.26431(15) 0.0346(4) Uani 1 1 d . .
H4A H 0.3372 0.3713 0.2452 0.042 Uiso 1 1 calc R U
H4B H 0.2692 0.4320 0.3386 0.042 Uiso 1 1 calc R U
N1 N 0.24709(18) 0.63094(14) 0.25222(13) 0.0285(4) Uani 1 1 d . .
C2 C 0.0712(2) 0.68658(14) 0.01769(12) 0.0243(4) Uani 1 1 d . .
C5 C -0.2085(2) 0.48702(16) 0.24383(14) 0.0329(4) Uani 1 1 d . .
H5A H -0.1808 0.4118 0.2631 0.039 Uiso 1 1 calc R U
H5B H -0.3112 0.4886 0.2272 0.039 Uiso 1 1 calc R U
C3 C 0.3511(2) 0.54082(17) 0.23529(16) 0.0375(5) Uani 1 1 d . .
H3A H 0.4387 0.5523 0.2783 0.045 Uiso 1 1 calc R U
H3B H 0.3747 0.5389 0.1631 0.045 Uiso 1 1 calc R U
C9 C 0.5962(2) 0.16564(17) -0.02539(16) 0.0386(5) Uani 1 1 d . .
C6 C -0.1689(2) 0.56587(16) 0.33137(14) 0.0349(4) Uani 1 1 d . .
H6A H -0.2116 0.6382 0.3174 0.042 Uiso 1 1 calc R U
H6B H -0.2029 0.5379 0.3960 0.042 Uiso 1 1 calc R U
C7 C 0.3741(2) 0.29560(18) -0.02130(16) 0.0429(5) Uani 1 1 d . .
H3N H 0.088(2) 0.3845(18) 0.2362(15) 0.035(6) Uiso 1 1 d . .
H4N H 0.150(2) 0.4172(16) 0.1406(17) 0.038(6) Uiso 1 1 d . .
H8N H 0.026(2) 0.5169(18) 0.3729(15) 0.035(6) Uiso 1 1 d . .
H5N H -0.177(2) 0.5775(17) 0.1220(15) 0.035(6) Uiso 1 1 d . .
H6N H -0.124(2) 0.4724(16) 0.1121(14) 0.041(6) Uiso 1 1 d D .
H2N H 0.266(2) 0.6846(16) 0.2191(14) 0.025(5) Uiso 1 1 d . .
H7N H 0.015(2) 0.6325(19) 0.3746(15) 0.036(6) Uiso 1 1 d . .
H1N H 0.245(2) 0.6466(18) 0.3178(17) 0.040(6) Uiso 1 1 d . .
H1O H 0.492(3) 0.263(2) -0.137(2) 0.085(9) 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'
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'
Co Co 0.3494 0.9721 '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
O2 Co1 O1 85.20(5)
O2 Co1 N4 175.47(6)
O1 Co1 N4 91.10(6)
O2 Co1 N3 91.29(6)
O1 Co1 N3 90.99(6)
N4 Co1 N3 86.14(6)
O2 Co1 N2 89.58(6)
O1 Co1 N2 174.11(6)
N4 Co1 N2 94.23(7)
N3 Co1 N2 91.85(7)
O2 Co1 N1 90.45(6)
O1 Co1 N1 91.58(6)
N4 Co1 N1 92.28(7)
N3 Co1 N1 177.01(7)
N2 Co1 N1 85.73(7)
C1 O1 Co1 112.94(10)
C2 O2 Co1 113.09(10)
C6 N4 Co1 108.98(10)
C4 N2 Co1 109.86(11)
C5 N3 Co1 109.94(11)
C9 C8 C7 119.84(19)
O4 C1 O1 124.95(16)
O4 C1 C2 121.16(14)
O1 C1 C2 113.87(14)
N2 C4 C3 106.70(14)
C3 N1 Co1 108.32(12)
O3 C2 O2 124.51(16)
O3 C2 C1 120.94(15)
O2 C2 C1 114.55(13)
N3 C5 C6 106.78(15)
N1 C3 C4 106.50(16)
O7 C9 O8 125.4(2)
O7 C9 C8 119.10(19)
O8 C9 C8 115.49(18)
N4 C6 C5 106.92(15)
O6 C7 O5 123.3(2)
O6 C7 C8 120.6(2)
O5 C7 C8 116.1(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 O2 1.9165(11)
Co1 O1 1.9225(11)
Co1 N4 1.9278(14)
Co1 N3 1.9419(15)
Co1 N2 1.9423(14)
Co1 N1 1.9532(16)
O6 C7 1.218(3)
O1 C1 1.2922(19)
O3 C2 1.2285(19)
O2 C2 1.2828(19)
O5 C7 1.285(2)
N4 C6 1.480(2)
O4 C1 1.221(2)
N2 C4 1.479(2)
O8 C9 1.295(2)
N3 C5 1.475(2)
C8 C9 1.501(3)
C8 C7 1.504(3)
O7 C9 1.210(2)
C1 C2 1.543(2)
C4 C3 1.499(3)
N1 C3 1.481(3)
C5 C6 1.504(3)
