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#$Date: 2024-11-29 04:02:58 +0200 (Fri, 29 Nov 2024) $
#$Revision: 296155 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249651.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_7249651
loop_
_publ_author_name
'Li, Xin'
'Zu, Mohan'
'Yan, Linzhuo'
'Zhao, Qiang'
'Liu, Liu'
_publ_section_title
;
 Synthesis of a highly stable Mo--Fe bimetallic metal--organic framework
 and its catalytic activity for the selective oxidation of sulfides under
 mild conditions
;
_journal_issue                   51
_journal_name_full               'RSC Advances'
_journal_page_first              38002
_journal_page_last               38008
_journal_paper_doi               10.1039/D4RA06324D
_journal_volume                  14
_journal_year                    2024
_chemical_formula_sum            'C20 H24 Fe4 Mo4 N4 O20'
_chemical_formula_weight         1247.59
_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   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2024-08-14 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                106.746(2)
_cell_angle_beta                 90.909(2)
_cell_angle_gamma                103.745(2)
_cell_formula_units_Z            1
_cell_length_a                   7.0109(12)
_cell_length_b                   9.4488(15)
_cell_length_c                   14.183(2)
_cell_measurement_reflns_used    2951
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      3.00
_cell_volume                     870.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4181
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.496
_diffrn_reflns_theta_max         24.496
_diffrn_reflns_theta_min         1.506
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       rod
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.5085
_refine_diff_density_max         1.755
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0444
_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)+(0.1090P)²+3.2496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2575
_reflns_number_total             2823
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra06324d2.cif
_cod_data_source_block           ddb
_cod_database_code               7249651
_shelx_shelxl_version_number     2017/1
_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_min   0.307
_shelx_estimated_absorpt_t_max   0.606
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_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
Mo1 Mo 0.37768(8) -0.00269(7) 0.11892(4) 0.0132(2) Uani 1 1 d . . . . .
Mo2 Mo 0.80314(8) -0.31350(6) -0.00258(4) 0.0123(2) Uani 1 1 d . . . . .
Fe1 Fe 0.29560(14) -0.33253(11) -0.07554(7) 0.0120(3) Uani 1 1 d . . . . .
Fe2 Fe 0.89639(14) 0.06573(11) 0.10076(7) 0.0137(3) Uani 1 1 d . . . . .
O1 O 0.0149(7) -0.2814(5) -0.0731(3) 0.0161(10) Uani 1 1 d . . . . .
O2 O 0.1958(7) -0.5289(6) -0.0367(4) 0.0205(11) Uani 1 1 d . . . . .
O3 O 0.5838(7) -0.3535(6) -0.0778(4) 0.0206(11) Uani 1 1 d . . . . .
O4 O 0.8163(8) -0.1567(6) 0.1044(4) 0.0204(11) Uani 1 1 d . . . . .
O5 O 0.6152(7) 0.1053(6) 0.0976(4) 0.0190(11) Uani 1 1 d . . . . .
O6 O 0.3655(9) 0.0477(6) 0.2433(4) 0.0299(13) Uani 1 1 d . . . . .
O7 O 0.3523(7) -0.2012(6) 0.0781(4) 0.0193(11) Uani 1 1 d . . . . .
O8 O 0.1775(7) 0.0419(6) 0.0617(3) 0.0165(10) Uani 1 1 d . . . . .
N1 N 0.2374(9) -0.4597(7) -0.2311(4) 0.0193(13) Uani 1 1 d . . . . .
N2 N -0.0203(9) -0.8355(7) -0.7451(4) 0.0187(13) Uani 1 1 d . . . . .
C1 C 0.1035(14) -0.5988(11) -0.2640(6) 0.040(2) Uani 1 1 d . . . . .
H1A H 0.039596 -0.641591 -0.218051 0.048 Uiso 1 1 calc R U . . .
C2 C 0.0605(14) -0.6774(10) -0.3631(6) 0.037(2) Uani 1 1 d . . . . .
H2A H -0.026986 -0.773700 -0.382036 0.044 Uiso 1 1 calc R U . . .
C3 C 0.1447(12) -0.6163(10) -0.4354(6) 0.0264(17) Uani 1 1 d . . . . .
C4 C 0.2829(12) -0.4755(11) -0.4004(6) 0.034(2) Uani 1 1 d . . . . .
H4A H 0.348455 -0.430222 -0.444977 0.041 Uiso 1 1 calc R U . . .
C5 C 0.3229(12) -0.4034(10) -0.3008(6) 0.0308(19) Uani 1 1 d . . . . .
H5A H 0.415192 -0.309330 -0.280443 0.037 Uiso 1 1 calc R U . . .
C6 C -0.0936(14) -0.8985(10) -0.6765(6) 0.034(2) Uani 1 1 d . . . . .
H6A H -0.183269 -0.993692 -0.698016 0.041 Uiso 1 1 calc R U . . .
C7 C -0.0480(15) -0.8351(11) -0.5785(6) 0.040(2) Uani 1 1 d . . . . .
H7A H -0.108978 -0.884808 -0.534972 0.049 Uiso 1 1 calc R U . . .
C8 C 0.0910(12) -0.6947(10) -0.5420(6) 0.0279(18) Uani 1 1 d . . . . .
C9 C 0.1726(12) -0.6292(10) -0.6134(6) 0.0279(18) Uani 1 1 d . . . . .
H9A H 0.268541 -0.536934 -0.594204 0.034 Uiso 1 1 calc R U . . .
C10 C 0.1120(12) -0.7002(10) -0.7122(6) 0.0298(19) Uani 1 1 d . . . . .
H10A H 0.165289 -0.652128 -0.757935 0.036 Uiso 1 1 calc R U . . .
O3W O 0.313(2) 0.0115(15) 0.4323(8) 0.041(3) Uani 0.5 1 d . . P A 1
H3WC H 0.416184 0.006605 0.462303 0.050 Uiso 0.5 1 d R U P A 1
H3WD H 0.341224 0.022365 0.376363 0.050 Uiso 0.5 1 d R U P A 1
O2W O 0.559(2) 0.2453(18) 0.5696(10) 0.048(3) Uani 0.5 1 d . . P B 2
H2WB H 0.568400 0.277537 0.632436 0.057 Uiso 0.5 1 d R U P B 2
H2WD H 0.441380 0.192887 0.549616 0.057 Uiso 0.5 1 d R U P B 2
O1W O 0.4221(18) -0.3470(11) 0.2253(7) 0.094(4) Uani 1 1 d . . . . .
H1WC H 0.402542 -0.294961 0.187865 0.113 Uiso 1 1 d R U . . .
H1WD H 0.423022 -0.435801 0.189005 0.113 Uiso 1 1 d R 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
_geom_angle_publ_flag
O6 Mo1 O7 107.2(3) . . ?
O6 Mo1 O8 109.2(2) . . ?
O7 Mo1 O8 109.6(2) . . ?
O6 Mo1 O5 106.6(3) . . ?
O7 Mo1 O5 112.6(2) . . ?
O8 Mo1 O5 111.5(2) . . ?
O2 Mo2 O3 108.5(2) 2_645 . ?
O2 Mo2 O4 107.4(2) 2_645 . ?
O3 Mo2 O4 111.0(2) . . ?
O2 Mo2 O1 107.8(2) 2_645 1_655 ?
O3 Mo2 O1 110.2(2) . 1_655 ?
O4 Mo2 O1 111.9(2) . 1_655 ?
O2 Fe1 O3 92.8(2) . . ?
O2 Fe1 O1 94.3(2) . . ?
O3 Fe1 O1 172.6(2) . . ?
O2 Fe1 O7 90.12(19) . . ?
O3 Fe1 O7 90.31(19) . . ?
O1 Fe1 O7 87.76(18) . . ?
O2 Fe1 N1 91.2(2) . . ?
O3 Fe1 N1 90.3(2) . . ?
O1 Fe1 N1 91.5(2) . . ?
O7 Fe1 N1 178.5(2) . . ?
O2 Fe1 O5 171.6(2) . 2_655 ?
O3 Fe1 O5 91.76(19) . 2_655 ?
O1 Fe1 O5 80.95(18) . 2_655 ?
O7 Fe1 O5 82.86(19) . 2_655 ?
N1 Fe1 O5 95.8(2) . 2_655 ?
O4 Fe2 O5 98.6(2) . . ?
O4 Fe2 O8 90.6(2) . 1_655 ?
O5 Fe2 O8 161.97(19) . 1_655 ?
O4 Fe2 N2 95.7(2) . 1_666 ?
O5 Fe2 N2 98.7(2) . 1_666 ?
O8 Fe2 N2 95.8(2) 1_655 1_666 ?
O4 Fe2 O1 171.01(19) . 2_655 ?
O5 Fe2 O1 83.45(19) . 2_655 ?
O8 Fe2 O1 85.13(18) 1_655 2_655 ?
N2 Fe2 O1 92.6(2) 1_666 2_655 ?
O4 Fe2 O8 83.57(19) . 2_655 ?
O5 Fe2 O8 84.14(18) . 2_655 ?
O8 Fe2 O8 81.55(18) 1_655 2_655 ?
N2 Fe2 O8 177.2(2) 1_666 2_655 ?
O1 Fe2 O8 87.97(18) 2_655 2_655 ?
Mo2 O1 Fe1 134.8(2) 1_455 . ?
Mo2 O1 Fe2 117.8(2) 1_455 2_655 ?
Fe1 O1 Fe2 98.2(2) . 2_655 ?
Mo2 O2 Fe1 160.5(3) 2_645 . ?
Mo2 O3 Fe1 143.1(3) . . ?
Mo2 O4 Fe2 122.0(3) . . ?
Mo1 O5 Fe2 131.5(3) . . ?
Mo1 O5 Fe1 130.9(3) . 2_655 ?
Fe2 O5 Fe1 97.30(19) . 2_655 ?
Mo1 O7 Fe1 122.6(3) . . ?
Mo1 O8 Fe2 134.6(3) . 1_455 ?
Mo1 O8 Fe2 117.6(2) . 2_655 ?
Fe2 O8 Fe2 98.45(18) 1_455 2_655 ?
C5 N1 C1 116.1(7) . . ?
C5 N1 Fe1 121.9(5) . . ?
C1 N1 Fe1 121.9(5) . . ?
C6 N2 C10 116.1(7) . . ?
C6 N2 Fe2 124.2(5) . 1_444 ?
C10 N2 Fe2 119.6(5) . 1_444 ?
N1 C1 C2 122.1(8) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C1 C2 C3 121.6(8) . . ?
C1 C2 H2A 119.2 . . ?
C3 C2 H2A 119.2 . . ?
C2 C3 C4 115.4(7) . . ?
C2 C3 C8 122.3(8) . . ?
C4 C3 C8 122.3(7) . . ?
C5 C4 C3 120.5(8) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
N1 C5 C4 124.2(8) . . ?
N1 C5 H5A 117.9 . . ?
C4 C5 H5A 117.9 . . ?
N2 C6 C7 125.1(8) . . ?
N2 C6 H6A 117.5 . . ?
C7 C6 H6A 117.5 . . ?
C6 C7 C8 120.0(8) . . ?
C6 C7 H7A 120.0 . . ?
C8 C7 H7A 120.0 . . ?
C9 C8 C7 115.4(7) . . ?
C9 C8 C3 121.4(8) . . ?
C7 C8 C3 123.1(8) . . ?
C10 C9 C8 120.4(8) . . ?
C10 C9 H9A 119.8 . . ?
C8 C9 H9A 119.8 . . ?
N2 C10 C9 122.9(8) . . ?
N2 C10 H10A 118.6 . . ?
C9 C10 H10A 118.6 . . ?
H3WC O3W H3WD 108.6 . . ?
H2WB O2W H2WD 108.3 . . ?
H1WC O1W H1WD 108.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O6 1.699(5) . ?
Mo1 O7 1.760(5) . ?
Mo1 O8 1.802(5) . ?
Mo1 O5 1.814(5) . ?
Mo2 O2 1.735(5) 2_645 ?
Mo2 O3 1.757(5) . ?
Mo2 O4 1.772(5) . ?
Mo2 O1 1.818(5) 1_655 ?
Fe1 O2 2.054(5) . ?
Fe1 O3 2.077(5) . ?
Fe1 O1 2.134(5) . ?
Fe1 O7 2.150(5) . ?
Fe1 N1 2.165(6) . ?
Fe1 O5 2.203(5) 2_655 ?
Fe2 O4 2.059(5) . ?
Fe2 O5 2.094(5) . ?
Fe2 O8 2.101(5) 1_655 ?
Fe2 N2 2.125(6) 1_666 ?
Fe2 O1 2.136(5) 2_655 ?
Fe2 O8 2.230(5) 2_655 ?
N1 C5 1.338(11) . ?
N1 C1 1.369(11) . ?
N2 C6 1.330(11) . ?
N2 C10 1.338(11) . ?
C1 C2 1.376(12) . ?
C1 H1A 0.9300 . ?
C2 C3 1.391(13) . ?
C2 H2A 0.9300 . ?
C3 C4 1.395(12) . ?
C3 C8 1.477(11) . ?
C4 C5 1.371(12) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.345(12) . ?
C6 H6A 0.9300 . ?
C7 C8 1.397(12) . ?
C7 H7A 0.9300 . ?
C8 C9 1.395(12) . ?
C9 C10 1.377(11) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
O3W H3WC 0.8500 . ?
O3W H3WD 0.8499 . ?
O2W H2WB 0.8500 . ?
O2W H2WD 0.8500 . ?
O1W H1WC 0.8502 . ?
O1W H1WD 0.8500 . ?
