#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:18:05 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229060 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/02/7230277.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_7230277
loop_
_publ_author_name
'Cindrić, Marina'
'Stilinović, Vladimir'
'Rubčić, Mirta'
'Medak, Glorija'
'Šišak Jung, Dubravka'
'Vrdoljak, Višnja'
_publ_section_title
;
 Supramolecular assembly of oxalatomolybdates controlled by the hydrogen
 bonding potential of Co(iii)-ammine cations
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1889
_journal_paper_doi               10.1039/C7CE02205K
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C2 H19 Co Mo N6 O11'
_chemical_formula_weight         458.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-02-01 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.0371(12)
_cell_length_b                   7.9845(3)
_cell_length_c                   6.4776(3)
_cell_measurement_reflns_used    6943
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      41.0626
_cell_measurement_theta_min      3.8711
_cell_volume                     1398.37(10)
_computing_structure_refinement  'SHELXL-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 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9126
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.874
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51457
_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            orange
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0223
_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)+(0.0381P)²+0.1737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1468
_reflns_number_total             1628
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce02205k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7230277--7230284.cif.'
_cod_database_code               7230277
_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
O4 O 0.13804(8) 0.7500 0.2762(3) 0.0241(4) Uani 1 2 d S T P
N4 N 0.20661(9) 0.2500 0.5985(4) 0.0237(5) Uani 1 2 d S T P
O5 O -0.02371(6) 0.5762(2) 0.3006(3) 0.0392(4) Uani 1 1 d . . .
C1 C 0.01160(7) 0.6522(3) 0.2323(3) 0.0232(4) Uani 1 1 d . . .
O7 O 0.25034(10) 0.2500 0.5557(4) 0.0482(7) Uani 1 2 d S T P
O6 O 0.19087(10) 0.2500 0.7717(4) 0.0462(7) Uani 1 2 d S T P
O8 O 0.29441(10) 0.2500 0.0990(5) 0.0523(8) Uani 1 2 d S T P
H11 H 0.314(2) 0.2500 0.015(9) 0.078 Uiso 1 2 d S U P
H10 H 0.311(2) 0.2500 0.200(9) 0.078 Uiso 1 2 d S U P
Mo1 Mo 0.10879(2) 0.7500 0.03530(4) 0.01686(9) Uani 1 2 d S T P
O3 O 0.05088(5) 0.58702(18) 0.1574(2) 0.0256(3) Uani 1 1 d . . .
O1 O 0.13453(6) 0.57721(19) -0.0871(2) 0.0269(3) Uani 1 1 d . . .
O2 O 0.05299(10) 0.7500 -0.2282(4) 0.0363(6) Uani 1 2 d S T P
H9 H 0.0356(11) 0.836(4) -0.247(5) 0.054 Uiso 1 1 d . U .
Co1 Co 0.15922(2) 0.2500 0.36657(6) 0.01580(11) Uani 1 2 d S T P
N1 N 0.11120(11) 0.2500 0.1343(4) 0.0243(6) Uani 1 2 d S T P
H1 H 0.1263(16) 0.2500 0.014(6) 0.037 Uiso 1 2 d S U P
H2 H 0.0966(10) 0.166(3) 0.127(4) 0.037 Uiso 1 1 d . U .
N3 N 0.19902(7) 0.4220(2) 0.2281(3) 0.0253(4) Uani 1 1 d . . .
H3 H 0.2264(11) 0.394(3) 0.200(4) 0.038 Uiso 1 1 d . U .
H4 H 0.1823(10) 0.465(4) 0.117(4) 0.038 Uiso 1 1 d . U .
H5 H 0.2015(9) 0.512(4) 0.302(4) 0.038 Uiso 1 1 d . U .
N2 N 0.12030(7) 0.4228(3) 0.5039(3) 0.0225(4) Uani 1 1 d . . .
H7 H 0.1169(9) 0.516(4) 0.430(4) 0.034 Uiso 1 1 d . U .
H6 H 0.1292(10) 0.452(4) 0.611(5) 0.034 Uiso 1 1 d . U .
H8 H 0.0908(11) 0.398(4) 0.522(4) 0.034 Uiso 1 1 d . U .
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'
Mo Mo -1.6832 0.6857 '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
O6 N4 O7 124.0(3) . .
O6 N4 Co1 118.8(2) . .
O7 N4 Co1 117.2(2) . .
O5 C1 O3 126.0(2) . .
O5 C1 C1 120.00(13) . 8_575
O3 C1 C1 114.04(11) . 8_575
O1 Mo1 O1 105.19(11) . 8_575
O1 Mo1 O4 103.07(7) . .
O1 Mo1 O4 103.07(7) 8_575 .
O1 Mo1 O3 88.81(6) . .
O1 Mo1 O3 157.80(7) 8_575 .
O4 Mo1 O3 90.06(7) . .
O1 Mo1 O3 157.79(7) . 8_575
O1 Mo1 O3 88.82(6) 8_575 8_575
O4 Mo1 O3 90.06(7) . 8_575
O3 Mo1 O3 73.14(8) . 8_575
O1 Mo1 O2 85.60(7) . .
O1 Mo1 O2 85.60(7) 8_575 .
O4 Mo1 O2 165.40(10) . .
O3 Mo1 O2 78.26(7) . .
O3 Mo1 O2 78.26(7) 8_575 .
C1 O3 Mo1 119.36(13) . .
N2 Co1 N2 90.06(12) . 8_565
N2 Co1 N3 90.54(9) . .
N2 Co1 N3 179.34(9) 8_565 .
N2 Co1 N3 179.33(9) . 8_565
N2 Co1 N3 90.55(9) 8_565 8_565
N3 Co1 N3 88.85(12) . 8_565
N2 Co1 N4 90.17(8) . .
N2 Co1 N4 90.18(8) 8_565 .
N3 Co1 N4 89.55(8) . .
N3 Co1 N4 89.55(8) 8_565 .
N2 Co1 N1 89.59(9) . .
N2 Co1 N1 89.59(9) 8_565 .
N3 Co1 N1 90.69(9) . .
N3 Co1 N1 90.70(9) 8_565 .
N4 Co1 N1 179.66(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O4 Mo1 1.750(2) .
N4 O6 1.200(4) .
N4 O7 1.215(4) .
N4 Co1 1.975(3) .
O5 C1 1.215(3) .
C1 O3 1.279(2) .
C1 C1 1.561(4) 8_575
Mo1 O1 1.7368(15) .
Mo1 O1 1.7368(15) 8_575
Mo1 O3 2.1842(14) .
Mo1 O3 2.1842(14) 8_575
Mo1 O2 2.278(2) .
Co1 N2 1.9497(19) .
Co1 N2 1.9497(19) 8_565
Co1 N3 1.9615(18) .
Co1 N3 1.9615(18) 8_565
Co1 N1 1.988(3) .
