#------------------------------------------------------------------------------
#$Date: 2019-11-23 00:28:56 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231659 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/62/4346204.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_4346204
loop_
_publ_author_name
'Luo, Lan'
'Zeng, Yuhan'
'Li, Le'
'Luo, Zhixiang'
'Smirnova, Tatyana I.'
'Maggard, Paul A.'
_publ_section_title
;
 Manganese-Vanadate Hybrids: Impact of Organic Ligands on Their
 Structures, Thermal Stabilities, Optical Properties, and Photocatalytic
 Activities.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7388
_journal_page_last               7401
_journal_paper_doi               10.1021/acs.inorgchem.5b00931
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C15 H11 Mn N3 O6 V2, H2 O'
_chemical_formula_sum            'C15 H13 Mn N3 O7 V2'
_chemical_formula_weight         504.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                106.749(14)
_cell_angle_beta                 102.050(14)
_cell_angle_gamma                106.448(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9073(12)
_cell_length_b                   11.2110(19)
_cell_length_c                   13.094(3)
_cell_measurement_reflns_used    4315
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      3.15
_cell_volume                     883.5(3)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9425
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0917 before and 0.0425 after correction.
The Ratio of minimum to maximum transmission is 0.8695.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             502
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3072
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0388
_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)+(0.0614P)²+1.1605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                2608
_reflns_number_total             3072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00931_si_003.cif
_cod_data_source_block           rds149_0ma_a
_cod_database_code               4346204
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Free rotating group:
 O00C(H00A,H00B)
3.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-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
Mn01 Mn 0.94993(8) 0.74716(5) 0.76906(4) 0.00709(15) Uani 1 1 d U
V002 V 1.49479(9) 1.17910(6) 1.15093(5) 0.00811(17) Uani 1 1 d U
V003 V 1.33950(9) 1.06943(5) 0.87054(5) 0.00827(17) Uani 1 1 d U
O004 O 1.7450(4) 1.2758(2) 1.2169(2) 0.0121(5) Uani 1 1 d U
O005 O 1.3480(4) 1.2334(2) 1.2246(2) 0.0102(5) Uani 1 1 d U
O006 O 1.4720(4) 1.0139(2) 1.1452(2) 0.0130(5) Uani 1 1 d U
O007 O 1.4205(4) 1.1823(2) 1.0131(2) 0.0156(6) Uani 1 1 d U
O008 O 1.3356(4) 1.1502(2) 0.7869(2) 0.0162(6) Uani 1 1 d U
N009 N 0.7838(4) 0.5327(3) 0.6730(2) 0.0090(6) Uani 1 1 d U
O00A O 1.0982(4) 0.9527(2) 0.8329(2) 0.0159(6) Uani 1 1 d U
N00B N 0.9088(5) 0.6501(3) 0.8944(3) 0.0104(6) Uani 1 1 d U
O00C O 0.7815(5) 1.0409(3) 0.7063(3) 0.0272(7) Uani 1 1 d G
H00A H 0.6859 1.0219 0.7391 0.041 Uiso 1 1 d G
H00B H 0.8919 1.0253 0.7363 0.041 Uiso 1 1 d G
N00D N 0.9062(5) 0.7141(3) 0.5859(3) 0.0112(6) Uani 1 1 d U
C00E C 0.7411(5) 0.4840(3) 0.5621(3) 0.0101(7) Uani 1 1 d U
C00F C 0.7820(5) 0.5186(3) 0.8510(3) 0.0094(7) Uani 1 1 d U
C00G C 0.7289(5) 0.4500(3) 0.7279(3) 0.0107(7) Uani 1 1 d U
C00H C 0.8081(5) 0.5868(3) 0.5124(3) 0.0111(7) Uani 1 1 d U
C00I C 0.9658(6) 0.7169(4) 1.0051(3) 0.0134(8) Uani 1 1 d U
H00I H 1.0545 0.8089 1.0354 0.016 Uiso 1 1 calc R
C00J C 0.7717(6) 0.5544(4) 0.3976(3) 0.0158(8) Uani 1 1 d U
H00J H 0.7016 0.4641 0.3467 0.019 Uiso 1 1 calc R
C00K C 0.6326(6) 0.3119(4) 0.6708(3) 0.0145(8) Uani 1 1 d U
H00K H 0.5987 0.2537 0.7101 0.017 Uiso 1 1 calc R
C00L C 0.8396(6) 0.6563(4) 0.3590(3) 0.0188(8) Uani 1 1 d U
H00L H 0.8152 0.6366 0.2808 0.023 Uiso 1 1 calc R
C00M C 0.9738(6) 0.8114(4) 0.5473(3) 0.0149(8) Uani 1 1 d U
H00M H 1.0457 0.9010 0.5996 0.018 Uiso 1 1 calc R
C00N C 0.7682(6) 0.5246(4) 1.0329(3) 0.0157(8) Uani 1 1 d U
H00N H 0.7194 0.4819 1.0806 0.019 Uiso 1 1 calc R
C00O C 0.5876(6) 0.2616(4) 0.5552(3) 0.0166(8) Uani 1 1 d U
H00O H 0.5198 0.1679 0.5143 0.020 Uiso 1 1 calc R
C00P C 0.7068(6) 0.4544(4) 0.9189(3) 0.0149(8) Uani 1 1 d U
H00P H 0.6142 0.3631 0.8871 0.018 Uiso 1 1 calc R
C00Q C 0.6407(6) 0.3468(4) 0.4991(3) 0.0151(8) Uani 1 1 d U
H00Q H 0.6098 0.3130 0.4198 0.018 Uiso 1 1 calc R
C00R C 0.9431(6) 0.7867(4) 0.4342(3) 0.0189(8) Uani 1 1 d U
H00R H 0.9919 0.8577 0.4090 0.023 Uiso 1 1 calc R
C00S C 0.9008(6) 0.6573(4) 1.0773(3) 0.0144(8) Uani 1 1 d U
H00S H 0.9467 0.7069 1.1558 0.017 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
O004 Mn01 N009 90.59(10) 2_877 .
O004 Mn01 N00B 89.05(10) 2_877 .
O004 Mn01 N00D 88.54(10) 2_877 .
O005 Mn01 O004 172.66(10) 2_777 2_877
O005 Mn01 N009 89.78(10) 2_777 .
O005 Mn01 N00B 84.03(10) 2_777 .
O005 Mn01 N00D 98.56(10) 2_777 .
N009 Mn01 N00B 73.44(11) . .
N009 Mn01 N00D 72.55(11) . .
O00A Mn01 O004 90.63(10) . 2_877
O00A Mn01 O005 90.27(9) . 2_777
O00A Mn01 N009 170.07(11) . .
O00A Mn01 N00B 116.43(11) . .
O00A Mn01 N00D 97.63(11) . .
N00B Mn01 N00D 145.88(11) . .
O004 V002 O005 108.57(12) . .
O004 V002 O006 106.83(12) . .
O004 V002 O007 109.34(13) . .
O005 V002 O006 109.69(12) . .
O005 V002 O007 111.26(12) . .
O007 V002 O006 111.02(12) . .
O007 V003 O006 109.06(12) . 2_877
O008 V003 O006 108.76(13) . 2_877
O008 V003 O007 110.26(13) . .
O008 V003 O00A 108.48(14) . .
O00A V003 O006 108.34(12) . 2_877
O00A V003 O007 111.88(13) . .
V002 O004 Mn01 136.07(13) . 2_877
V002 O005 Mn01 149.79(15) . 2_777
V002 O006 V003 129.38(13) . 2_877
V002 O007 V003 138.32(15) . .
C00E N009 Mn01 120.4(2) . .
C00E N009 C00G 120.4(3) . .
C00G N009 Mn01 119.1(2) . .
V003 O00A Mn01 139.79(14) . .
C00F N00B Mn01 115.7(2) . .
C00I N00B Mn01 124.3(2) . .
C00I N00B C00F 118.8(3) . .
C00H N00D Mn01 116.6(2) . .
C00M N00D Mn01 124.5(2) . .
C00M N00D C00H 118.9(3) . .
N009 C00E C00H 114.6(3) . .
N009 C00E C00Q 121.6(3) . .
C00Q C00E C00H 123.8(3) . .
N00B C00F C00G 115.9(3) . .
N00B C00F C00P 121.2(3) . .
C00P C00F C00G 122.9(3) . .
N009 C00G C00F 114.5(3) . .
N009 C00G C00K 121.0(3) . .
C00K C00G C00F 124.5(3) . .
N00D C00H C00E 115.7(3) . .
N00D C00H C00J 121.7(3) . .
C00J C00H C00E 122.6(3) . .
N00B C00I C00S 122.6(3) . .
C00L C00J C00H 118.6(4) . .
C00O C00K C00G 118.3(4) . .
C00R C00L C00J 119.9(4) . .
N00D C00M C00R 122.6(4) . .
C00S C00N C00P 119.5(3) . .
C00Q C00O C00K 120.4(3) . .
C00N C00P C00F 119.2(3) . .
C00O C00Q C00E 118.2(4) . .
C00L C00R C00M 118.3(4) . .
C00N C00S C00I 118.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn01 O004 2.171(2) 2_877
Mn01 O005 2.146(2) 2_777
Mn01 N009 2.185(3) .
Mn01 O00A 2.062(2) .
Mn01 N00B 2.238(3) .
Mn01 N00D 2.258(3) .
V002 O004 1.638(2) .
V002 O005 1.658(2) .
V002 O006 1.792(2) .
V002 O007 1.784(3) .
V003 O006 1.816(2) 2_877
V003 O007 1.789(3) .
V003 O008 1.610(3) .
V003 O00A 1.669(3) .
O004 Mn01 2.171(2) 2_877
O005 Mn01 2.146(2) 2_777
O006 V003 1.816(2) 2_877
N009 C00E 1.329(5) .
N009 C00G 1.349(5) .
N00B C00F 1.357(5) .
N00B C00I 1.336(5) .
N00D C00H 1.345(5) .
N00D C00M 1.340(5) .
C00E C00H 1.491(5) .
C00E C00Q 1.398(5) .
C00F C00G 1.484(5) .
C00F C00P 1.389(5) .
C00G C00K 1.393(5) .
C00H C00J 1.391(5) .
C00I C00S 1.383(5) .
C00J C00L 1.381(6) .
C00K C00O 1.384(6) .
C00L C00R 1.380(6) .
C00M C00R 1.383(6) .
C00N C00P 1.378(6) .
C00N C00S 1.377(5) .
C00O C00Q 1.380(6) .
