#------------------------------------------------------------------------------
#$Date: 2019-11-23 00:28:39 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231658 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/62/4346203.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_4346203
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         'C4 H3.61 Mn N2 O6.31 V2'
_chemical_formula_sum            'C4 H3.61 Mn N2 O6.31 V2'
_chemical_formula_weight         337.41
_chemical_name_systematic        Mn2(bipym)V4O12
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2014-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.581(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3490(4)
_cell_length_b                   18.9527(10)
_cell_length_c                   5.9129(3)
_cell_measurement_temperature    110(2)
_cell_volume                     931.20(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.605
_diffrn_reflns_theta_min         2.149
_exptl_absorpt_coefficient_mu    3.313
_exptl_absorpt_correction_T_max  0.9367
_exptl_absorpt_correction_T_min  0.8259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.407
_exptl_crystal_description       block
_exptl_crystal_F_000             652.2
_exptl_crystal_preparation       hydrothermal
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0292P)²+3.4163P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                905
_reflns_number_total             1117
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00931_si_002.cif
_cod_data_source_block           rds115_0m_a
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4346203
_shelxl_version_number           2014/6
_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.
;
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.826
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(1)
3.a Free rotating group:
 O5(H5A,H5B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Mn1 Mn 0.0000 0.65857(4) 1.0000 0.00935(19) Uani 1 2 d S T P
V1 V -0.09954(7) 0.81716(3) 1.23259(9) 0.01011(17) Uani 1 1 d . . .
O1 O -0.1046(3) 0.72999(13) 1.2108(4) 0.0150(5) Uani 1 1 d . . .
O2 O 0.0000 0.85209(18) 1.0000 0.0143(7) Uani 1 2 d S T P
O3 O -0.2845(3) 0.84841(13) 1.2162(4) 0.0146(5) Uani 1 1 d . . .
O4 O 0.0000 0.84474(18) 1.5000 0.0129(7) Uani 1 2 d S T P
N1 N 0.0940(3) 0.56252(15) 0.8265(4) 0.0092(6) Uani 1 1 d . . .
C1 C 0.1897(4) 0.5622(2) 0.6580(6) 0.0127(7) Uani 1 1 d . . .
C3 C 0.0522(5) 0.5000 0.9057(7) 0.0080(9) Uani 1 2 d S T P
O5 O 0.5797(16) 0.5000 0.901(2) 0.021(4) Uani 0.305(12) 2 d S T P
H5A H 0.5309 0.4645 0.9575 0.031 Uiso 0.153(6) 1 d G . .
H5B H 0.5732 0.5367 0.9880 0.031 Uiso 0.153(6) 1 d G . .
C0AA C 0.2408(6) 0.5000 0.5672(9) 0.0165(11) Uani 1 2 d S T P
H0AA H 0.306(7) 0.5000 0.459(10) 0.020 Uiso 1 2 d RS T P
H1 H 0.213(4) 0.605(2) 0.598(6) 0.020 Uiso 1 1 d 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'
Mn Mn 0.3368 0.7283 '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'
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
O1 Mn1 O1 99.18(13) 2_557 .
O1 Mn1 O3 91.19(9) 2_557 8_565
O1 Mn1 O3 93.47(9) 2_557 7_467
O1 Mn1 O3 93.47(9) . 8_565
O1 Mn1 O3 91.19(9) . 7_467
O1 Mn1 N1 93.85(9) . 2_557
O1 Mn1 N1 93.85(9) 2_557 .
O1 Mn1 N1 166.90(10) 2_557 2_557
O1 Mn1 N1 166.90(10) . .
O3 Mn1 O3 172.80(14) 7_467 8_565
O3 Mn1 N1 89.30(9) 8_565 2_557
O3 Mn1 N1 89.30(9) 7_467 .
O3 Mn1 N1 84.91(9) 8_565 .
O3 Mn1 N1 84.91(9) 7_467 2_557
N1 Mn1 N1 73.15(14) 2_557 .
O1 V1 O2 108.50(13) . .
O1 V1 O4 111.45(13) . .
O3 V1 O1 109.70(12) . .
O3 V1 O2 108.80(10) . .
O3 V1 O4 107.39(10) . .
O4 V1 O2 110.97(8) . .
V1 O1 Mn1 133.13(13) . .
V1 O2 V1 136.9(2) 2_557 .
V1 O3 Mn1 138.86(13) . 7_467
V1 O4 V1 146.1(2) 2_558 .
C1 N1 Mn1 126.9(2) . .
C3 N1 Mn1 116.2(2) . .
C3 N1 C1 116.9(3) . .
N1 C1 C0AA 121.6(4) . .
N1 C3 N1 125.5(4) . 6_565
N1 C3 C3 117.3(2) . 5_567
N1 C3 C3 117.3(2) 6_565 5_567
C1 C0AA C1 117.3(5) 6_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.088(2) 2_557
Mn1 O1 2.088(2) .
Mn1 O3 2.107(2) 7_467
Mn1 O3 2.107(2) 8_565
Mn1 N1 2.267(3) 2_557
Mn1 N1 2.267(3) .
V1 O1 1.657(2) .
V1 O2 1.8007(14) .
V1 O3 1.648(2) .
V1 O4 1.7912(11) .
O2 V1 1.8007(13) 2_557
O3 Mn1 2.107(2) 7_467
O4 V1 1.7912(11) 2_558
N1 C1 1.336(4) .
N1 C3 1.333(3) .
C1 C0AA 1.379(5) .
C3 N1 1.333(3) 6_565
C3 C3 1.480(9) 5_567
C0AA C1 1.379(5) 6_565
