#------------------------------------------------------------------------------
#$Date: 2022-02-22 12:50:10 +0200 (Tue, 22 Feb 2022) $
#$Revision: 273108 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/46/8104604.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_8104604
loop_
_publ_author_name
'Ze-Hai, Qiu'
'Zhu-Sen, Zhang'
'Wu-Hua, Chen'
_publ_section_title
;
 The crystal structure of catena-poly[(1,10-phenanthroline-k2
 N,N′)-(μ3-tetraoxidomoybdato(VI)-k3
 O:O′:O″)manganese(II)] C12H8N2O4MoMn
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1347
_journal_page_last               1349
_journal_paper_doi               10.1515/ncrs-2021-0338
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         '0.5(C24 H16 Mn2 Mo2 N4 O8)'
_chemical_formula_sum            'C12 H8 Mn Mo N2 O4'
_chemical_formula_weight         395.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 100.120(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9812(5)
_cell_length_b                   6.5212(3)
_cell_length_c                   10.6167(6)
_cell_measurement_reflns_used    1469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6100
_cell_measurement_theta_min      2.3130
_cell_volume                     612.13(6)
_computing_cell_refinement
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_data_collection
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_data_reduction
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)[2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[2]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[3]'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)[4]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1151
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -68.00 -35.00   1.00    1.21    --  -17.60-178.00-150.00   33
  2  ω    -46.00  48.00   1.00    1.21    --  -17.60  19.00  90.00   94
  3  ω    -73.00   1.00   1.00    1.21    --  -17.60 -38.00  60.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0457737000
_diffrn_orient_matrix_UB_12      0.0131169000
_diffrn_orient_matrix_UB_13      -0.0475085000
_diffrn_orient_matrix_UB_21      0.0579133000
_diffrn_orient_matrix_UB_22      -0.0592966000
_diffrn_orient_matrix_UB_23      0.0371551000
_diffrn_orient_matrix_UB_31      -0.0313674000
_diffrn_orient_matrix_UB_32      -0.0901258000
_diffrn_orient_matrix_UB_33      -0.0312753000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2729
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.272
_diffrn_reflns_theta_min         1.949
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent dark yellow'
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_description       cube
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0391
_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)+(0.0096P)²+1.7057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1342
_reflns_number_total             1520
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0338_suppl.cif
_cod_data_source_block           lym0912-d1
_cod_database_code               8104604
_chemical_oxdiff_formula         'C H N O Mo W Mn Co P V'
_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.
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim Mn1 \\sim Mo1: within 3.8A with sigma of 0.002 and sigma for terminal
atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.19766(9) 0.7500 0.16874(8) 0.0209(2) Uani 1 2 d S TU P . .
Mo1 Mo -0.00443(5) 0.2500 0.17991(4) 0.01716(14) Uani 1 2 d S TU P . .
C1 C 0.4663(7) 0.7500 0.0065(6) 0.0307(14) Uani 1 2 d S T P . .
H1 H 0.3891 0.7500 -0.0646 0.037 Uiso 1 2 calc RS T P . .
C2 C 0.6170(8) 0.7500 -0.0123(6) 0.0371(16) Uani 1 2 d S T P . .
H2 H 0.6377 0.7500 -0.0952 0.044 Uiso 1 2 calc RS T P . .
C3 C 0.7336(8) 0.7500 0.0888(6) 0.0356(15) Uani 1 2 d S T P . .
H3 H 0.8334 0.7500 0.0760 0.043 Uiso 1 2 calc RS T P . .
C4 C 0.6992(6) 0.7500 0.2142(6) 0.0266(13) Uani 1 2 d S T P . .
C5 C 0.8112(7) 0.7500 0.3289(6) 0.0365(16) Uani 1 2 d S T P . .
H5 H 0.9129 0.7500 0.3217 0.044 Uiso 1 2 calc RS T P . .
C6 C 0.7752(7) 0.7500 0.4441(6) 0.0332(15) Uani 1 2 d S T P . .
H6 H 0.8513 0.7500 0.5159 0.040 Uiso 1 2 calc RS T P . .
C7 C 0.6176(6) 0.7500 0.4599(6) 0.0228(12) Uani 1 2 d S T P . .
C8 C 0.5726(7) 0.7500 0.5803(6) 0.0249(12) Uani 1 2 d S T P . .
H8 H 0.6447 0.7500 0.6548 0.030 Uiso 1 2 calc RS T P . .
C9 C 0.4236(7) 0.7500 0.5868(6) 0.0302(14) Uani 1 2 d S T P . .
H9 H 0.3922 0.7500 0.6657 0.036 Uiso 1 2 calc RS T P . .
C10 C 0.3172(7) 0.7500 0.4731(6) 0.0269(13) Uani 1 2 d S T P . .
H10 H 0.2150 0.7500 0.4788 0.032 Uiso 1 2 calc RS T P . .
C11 C 0.5042(6) 0.7500 0.3515(5) 0.0202(11) Uani 1 2 d S T P . .
C12 C 0.5446(6) 0.7500 0.2258(5) 0.0202(11) Uani 1 2 d S T P . .
N1 N 0.4303(5) 0.7500 0.1223(4) 0.0226(10) Uani 1 2 d S T P . .
N2 N 0.3546(5) 0.7500 0.3588(5) 0.0212(10) Uani 1 2 d S T P . .
O1 O 0.1094(3) 0.4728(4) 0.2096(3) 0.0303(5) Uani 1 1 d . U . . .
O2 O -0.1344(6) 0.2500 0.2788(5) 0.0580(16) Uani 1 2 d S T P . .
O3 O -0.1010(6) 0.2500 0.0217(4) 0.0483(13) Uani 1 2 d S T P . .
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'
Mn Mn 0.3368 0.7283 '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
N1 Mn1 N2 74.60(17) . .
O1 Mn1 N1 117.32(8) . .
O1 Mn1 N1 117.32(8) 4_575 .
O1 Mn1 N2 90.85(10) . .
O1 Mn1 N2 90.85(10) 4_575 .
O1 Mn1 O1 123.65(17) . 4_575
O1 Mn1 O3 95.51(11) 4_575 3_565
O1 Mn1 O3 95.51(11) . 3_565
O3 Mn1 N1 91.9(2) 3_565 .
O3 Mn1 N2 166.5(2) 3_565 .
O1 Mo1 O1 110.09(18) 4_565 .
O2 Mo1 O1 109.09(14) . 4_565
O2 Mo1 O1 109.09(14) . .
O2 Mo1 O3 108.3(3) . .
O3 Mo1 O1 110.11(12) . 4_565
O3 Mo1 O1 110.11(13) . .
C2 C1 H1 119.0 . .
N1 C1 H1 119.0 . .
N1 C1 C2 122.1(6) . .
C1 C2 H2 119.5 . .
C3 C2 C1 121.0(6) . .
C3 C2 H2 119.5 . .
C2 C3 H3 120.8 . .
C2 C3 C4 118.4(6) . .
C4 C3 H3 120.8 . .
C3 C4 C5 124.1(6) . .
C12 C4 C3 117.4(5) . .
C12 C4 C5 118.5(6) . .
C4 C5 H5 118.8 . .
C6 C5 C4 122.4(6) . .
C6 C5 H5 118.8 . .
C5 C6 H6 119.7 . .
C5 C6 C7 120.6(6) . .
C7 C6 H6 119.7 . .
C8 C7 C6 123.1(5) . .
C11 C7 C6 119.2(5) . .
C11 C7 C8 117.7(5) . .
C7 C8 H8 120.3 . .
C9 C8 C7 119.4(5) . .
C9 C8 H8 120.3 . .
C8 C9 H9 120.4 . .
C8 C9 C10 119.2(6) . .
C10 C9 H9 120.4 . .
C9 C10 H10 118.4 . .
N2 C10 C9 123.3(6) . .
N2 C10 H10 118.4 . .
C7 C11 C12 119.8(5) . .
N2 C11 C7 122.5(5) . .
N2 C11 C12 117.7(5) . .
C4 C12 C11 119.3(5) . .
N1 C12 C4 122.7(5) . .
N1 C12 C11 118.0(5) . .
C1 N1 Mn1 126.6(4) . .
C1 N1 C12 118.4(5) . .
C12 N1 Mn1 115.0(4) . .
C10 N2 Mn1 127.3(4) . .
C10 N2 C11 117.9(5) . .
C11 N2 Mn1 114.7(4) . .
Mo1 O1 Mn1 156.51(16) . .
Mo1 O3 Mn1 175.4(3) . 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N1 2.230(5) .
Mn1 N2 2.249(5) .
Mn1 O1 2.051(3) .
Mn1 O1 2.051(3) 4_575
Mn1 O3 2.055(4) 3_565
Mo1 O1 1.773(3) 4_565
Mo1 O1 1.773(3) .
Mo1 O2 1.701(4) .
Mo1 O3 1.750(4) .
C1 H1 0.9300 .
C1 C2 1.403(9) .
C1 N1 1.325(7) .
C2 H2 0.9300 .
C2 C3 1.362(9) .
C3 H3 0.9300 .
C3 C4 1.418(8) .
C4 C5 1.437(8) .
C4 C12 1.416(8) .
C5 H5 0.9300 .
C5 C6 1.318(9) .
C6 H6 0.9300 .
C6 C7 1.455(8) .
C7 C8 1.407(8) .
C7 C11 1.397(8) .
C8 H8 0.9300 .
C8 C9 1.351(8) .
C9 H9 0.9300 .
C9 C10 1.402(8) .
C10 H10 0.9300 .
C10 N2 1.315(7) .
C11 C12 1.442(7) .
C11 N2 1.360(7) .
C12 N1 1.365(7) .
O3 Mn1 2.055(4) 3_565
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
C1 C2 C3 C4 0.000(0) . . . .
C2 C1 N1 Mn1 180.0 . . . .
C2 C1 N1 C12 0.000(0) . . . .
C2 C3 C4 C5 180.000(1) . . . .
C2 C3 C4 C12 0.000(1) . . . .
C3 C4 C5 C6 180.000(1) . . . .
C3 C4 C12 C11 180.000(1) . . . .
C3 C4 C12 N1 0.000(1) . . . .
C4 C5 C6 C7 0.000(1) . . . .
C4 C12 N1 Mn1 180.000(0) . . . .
C4 C12 N1 C1 0.000(0) . . . .
C5 C4 C12 C11 0.000(1) . . . .
C5 C4 C12 N1 180.000(1) . . . .
C5 C6 C7 C8 180.000(1) . . . .
C5 C6 C7 C11 0.000(1) . . . .
C6 C7 C8 C9 180.000(1) . . . .
C6 C7 C11 C12 0.000(1) . . . .
C6 C7 C11 N2 180.000(1) . . . .
C7 C8 C9 C10 0.000(2) . . . .
C7 C11 C12 C4 0.000(1) . . . .
C7 C11 C12 N1 180.000(1) . . . .
C7 C11 N2 Mn1 180.000(1) . . . .
C7 C11 N2 C10 0.000(1) . . . .
C8 C7 C11 C12 180.000(1) . . . .
C8 C7 C11 N2 0.000(1) . . . .
C8 C9 C10 N2 0.000(2) . . . .
C9 C10 N2 Mn1 180.000(1) . . . .
C9 C10 N2 C11 0.000(1) . . . .
C11 C7 C8 C9 0.000(2) . . . .
C11 C12 N1 Mn1 0.000(0) . . . .
C11 C12 N1 C1 180.000(1) . . . .
C12 C4 C5 C6 0.000(1) . . . .
C12 C11 N2 Mn1 0.000(1) . . . .
C12 C11 N2 C10 180.000(1) . . . .
N1 C1 C2 C3 0.000(0) . . . .
N2 C11 C12 C4 180.000(1) . . . .
N2 C11 C12 N1 0.000(1) . . . .
O1 Mo1 O1 Mn1 124.6(4) 4_565 . . .
O2 Mo1 O1 Mn1 -115.7(5) . . . .
O3 Mo1 O1 Mn1 3.1(5) . . . .
