#------------------------------------------------------------------------------
#$Date: 2021-09-06 13:05:03 +0200 (lun 06 de sep de 2021) $
#$Revision: 268740 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/78/7707844.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_7707844
loop_
_publ_author_name
'Zhou, Chuan-Cong'
'Liu, Hou-Ting'
'Ding, Li'
'Lu, Jing'
'Wang, Su-Na'
'Li, Yun-Wu'
_publ_section_title
;
 Single-crystal-to-single-crystal transformations among three Mn-MOFs
 containing different water molecules induced by reaction time: crystal
 structures and proton conductivities.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11077
_journal_page_last               11090
_journal_paper_doi               10.1039/d1dt01163d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C14 H17 Mn1.5 N O11.5'
_chemical_formula_weight         465.69
_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-2018/3
_audit_update_record
;
2021-03-04 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                103.790(8)
_cell_angle_beta                 100.798(8)
_cell_angle_gamma                101.414(8)
_cell_formula_units_Z            2
_cell_length_a                   6.8023(7)
_cell_length_b                   9.1613(8)
_cell_length_c                   14.8193(15)
_cell_measurement_reflns_used    1474
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.4340
_cell_measurement_theta_min      5.1320
_cell_volume                     852.06(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    diamond
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5020
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.247
_diffrn_reflns_theta_max         67.247
_diffrn_reflns_theta_min         5.140
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       block
_exptl_crystal_F_000             475
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.937
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3038
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0711
_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)+(0.1072P)²+2.1566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.2101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2355
_reflns_number_total             3038
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01163d2.cif
_cod_data_source_block           exp_10202
_cod_depositor_comments
'Adding full bibliography for 7707842--7707844.cif.'
_cod_original_cell_volume        852.05(15)
_cod_original_formula_sum        'C14 H17 Mn1.50 N O11.50'
_cod_database_code               7707844
_shelx_shelxl_version_number     2018/3
_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   0.385
_shelx_estimated_absorpt_t_max   0.411
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
Mn1 Mn 0.500000 1.000000 0.000000 0.0126(3) Uani 1 2 d S U P . .
Mn2 Mn 0.30483(17) 0.55766(11) 0.19560(7) 0.0233(3) Uani 1 1 d . U . . .
N1 N 0.5269(8) 0.7736(5) 0.3113(3) 0.0148(10) Uani 1 1 d . U . . .
O1 O 0.6743(9) 0.5633(5) 0.6879(4) 0.0396(13) Uani 1 1 d . U . . .
O2 O 0.8507(7) 0.7037(5) 0.8303(3) 0.0207(9) Uani 1 1 d . U . . .
O3 O 1.1530(7) 1.2846(5) 0.8839(3) 0.0274(11) Uani 1 1 d . U . . .
O4 O 0.9719(7) 1.3786(5) 0.7818(3) 0.0225(10) Uani 1 1 d . U . . .
O5 O 0.5319(7) 0.9881(4) 0.1424(3) 0.0194(9) Uani 1 1 d . U . . .
O6 O 0.3661(7) 0.7438(5) 0.1263(3) 0.0214(9) Uani 1 1 d . U . . .
O9 O 0.5196(9) 0.4738(5) 0.1202(4) 0.0434(14) Uani 1 1 d . U . . .
H9B H 0.634555 0.488893 0.159858 0.065 Uiso 1 1 d R U . . .
H9D H 0.537355 0.522953 0.079198 0.065 Uiso 1 1 d R U . . .
O10 O 0.0524(15) 0.4706(10) 0.0365(6) 0.028(2) Uani 0.5 1 d . U P . .
H10B H 0.028111 0.559360 0.041806 0.034 Uiso 0.5 1 d R U P . .
H10C H -0.014459 0.434500 -0.021954 0.034 Uiso 0.5 1 d R U P . .
O7 O 0.7473(7) 0.8813(5) -0.0088(3) 0.0251(10) Uani 1 1 d . U . . .
H7B H 0.741176 0.819379 0.025753 0.038 Uiso 1 1 d R U . . .
H7C H 0.732496 0.830169 -0.066687 0.038 Uiso 1 1 d R U . . .
O8 O 0.2741(7) 0.7693(5) -0.0592(3) 0.0248(10) Uani 1 1 d . U . . .
H8B H 0.152029 0.780980 -0.064125 0.037 Uiso 1 1 d R U . . .
H8D H 0.296149 0.713840 -0.021705 0.037 Uiso 1 1 d R U . . .
O11 O 0.2001(19) 0.5558(14) 0.6717(9) 0.145(4) Uani 1 1 d . U . . .
H11C H 0.112619 0.497330 0.690227 0.174 Uiso 1 1 d R U . . .
H11A H 0.317039 0.534840 0.682327 0.174 Uiso 1 1 d R U . . .
O12 O 0.864(2) 0.4355(15) 0.5245(10) 0.180(5) Uani 1 1 d . U . . .
H12C H 0.761148 0.454106 0.546034 0.216 Uiso 1 1 d R U . . .
H12D H 0.842218 0.438376 0.466654 0.216 Uiso 1 1 d R U . . .
C1 C 0.7803(10) 0.6914(7) 0.7437(4) 0.0196(12) Uani 1 1 d . U . . .
C2 C 0.8182(9) 0.8310(6) 0.7067(4) 0.0167(12) Uani 1 1 d . U . . .
C3 C 0.9155(9) 0.9768(6) 0.7720(4) 0.0147(11) Uani 1 1 d . U . . .
H3 H 0.965814 0.986730 0.836547 0.018 Uiso 1 1 calc R U . . .
C4 C 0.9352(9) 1.1070(6) 0.7380(4) 0.0132(11) Uani 1 1 d . U . . .
C5 C 0.8647(9) 1.0912(6) 0.6422(4) 0.0142(11) Uani 1 1 d . U . . .
H5 H 0.877370 1.179562 0.621009 0.017 Uiso 1 1 calc R U . . .
C6 C 0.7744(9) 0.9453(6) 0.5758(4) 0.0127(11) Uani 1 1 d . U . . .
C7 C 0.7482(9) 0.8151(6) 0.6102(4) 0.0174(12) Uani 1 1 d . U . . .
H7A H 0.683159 0.717148 0.567841 0.021 Uiso 1 1 calc R U . . .
C8 C 1.0262(9) 1.2669(6) 0.8064(4) 0.0148(11) Uani 1 1 d . U . . .
C9 C 0.7057(9) 0.9298(6) 0.4716(4) 0.0131(11) Uani 1 1 d . U . . .
C10 C 0.7459(9) 1.0582(7) 0.4362(4) 0.0176(12) Uani 1 1 d . U . . .
H10A H 0.819756 1.154624 0.478070 0.021 Uiso 1 1 calc R U . . .
C11 C 0.6780(9) 1.0440(6) 0.3402(4) 0.0146(11) Uani 1 1 d . U . . .
H11 H 0.705176 1.129275 0.316568 0.017 Uiso 1 1 calc R U . . .
C12 C 0.5678(9) 0.8988(6) 0.2799(4) 0.0130(11) Uani 1 1 d . U . . .
C13 C 0.5946(10) 0.7896(7) 0.4035(4) 0.0195(12) Uani 1 1 d . U . . .
H13 H 0.566393 0.701589 0.424595 0.023 Uiso 1 1 calc R U . . .
C14 C 0.4823(9) 0.8760(6) 0.1742(4) 0.0131(11) Uani 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 '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
O5 Mn1 O5 180.0 . 2_675 ?
O5 Mn1 O7 92.18(17) . 2_675 ?
O5 Mn1 O7 87.81(17) 2_675 2_675 ?
O5 Mn1 O7 87.82(17) . . ?
O5 Mn1 O7 92.18(17) 2_675 . ?
O7 Mn1 O7 180.00(19) 2_675 . ?
O5 Mn1 O8 92.61(16) . . ?
O5 Mn1 O8 87.39(16) 2_675 . ?
O7 Mn1 O8 91.74(17) 2_675 . ?
O7 Mn1 O8 88.26(17) . . ?
O5 Mn1 O8 87.39(16) . 2_675 ?
O5 Mn1 O8 92.61(16) 2_675 2_675 ?
O7 Mn1 O8 88.26(17) 2_675 2_675 ?
O7 Mn1 O8 91.74(17) . 2_675 ?
O8 Mn1 O8 180.0 . 2_675 ?
O4 Mn2 O9 159.2(2) 2_676 . ?
O4 Mn2 O6 89.13(17) 2_676 . ?
O9 Mn2 O6 82.07(19) . . ?
O4 Mn2 O1 93.8(2) 2_676 2_666 ?
O9 Mn2 O1 101.3(2) . 2_666 ?
O6 Mn2 O1 158.76(17) . 2_666 ?
O4 Mn2 N1 95.07(17) 2_676 . ?
O9 Mn2 N1 100.21(19) . . ?
O6 Mn2 N1 72.74(16) . . ?
O1 Mn2 N1 86.04(17) 2_666 . ?
O4 Mn2 O2 91.50(16) 2_676 2_666 ?
O9 Mn2 O2 85.08(17) . 2_666 ?
O6 Mn2 O2 144.68(15) . 2_666 ?
O1 Mn2 O2 56.37(16) 2_666 2_666 ?
N1 Mn2 O2 142.20(16) . 2_666 ?
C13 N1 C12 118.5(5) . . ?
C13 N1 Mn2 127.6(4) . . ?
C12 N1 Mn2 113.5(4) . . ?
C1 O1 Mn2 93.4(4) . 2_666 ?
C1 O2 Mn2 90.3(3) . 2_666 ?
C8 O4 Mn2 122.7(4) . 2_676 ?
C14 O5 Mn1 130.8(4) . . ?
C14 O6 Mn2 120.3(4) . . ?
O1 C1 O2 120.0(6) . . ?
O1 C1 C2 119.6(6) . . ?
O2 C1 C2 120.4(5) . . ?
C7 C2 C3 121.0(5) . . ?
C7 C2 C1 120.1(5) . . ?
C3 C2 C1 118.9(5) . . ?
C4 C3 C2 118.4(5) . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 C8 119.2(5) . . ?
C3 C4 C8 120.3(5) . . ?
C4 C5 C6 121.5(5) . . ?
C5 C6 C7 118.1(5) . . ?
C5 C6 C9 120.8(5) . . ?
C7 C6 C9 121.1(5) . . ?
C2 C7 C6 120.4(5) . . ?
O3 C8 O4 123.0(5) . . ?
O3 C8 C4 119.5(5) . . ?
O4 C8 C4 117.4(5) . . ?
C13 C9 C10 115.6(5) . . ?
C13 C9 C6 123.2(5) . . ?
C10 C9 C6 121.2(5) . . ?
C11 C10 C9 121.0(5) . . ?
C10 C11 C12 118.0(5) . . ?
N1 C12 C11 122.6(5) . . ?
N1 C12 C14 116.7(5) . . ?
C11 C12 C14 120.7(5) . . ?
N1 C13 C9 124.3(5) . . ?
O5 C14 O6 125.9(5) . . ?
O5 C14 C12 117.5(5) . . ?
O6 C14 C12 116.6(5) . . ?
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
Mn1 O5 2.112(4) . ?
Mn1 O5 2.112(4) 2_675 ?
Mn1 O7 2.184(4) 2_675 ?
Mn1 O7 2.184(4) . ?
Mn1 O8 2.219(4) . ?
Mn1 O8 2.219(4) 2_675 ?
Mn2 O4 2.139(4) 2_676 ?
Mn2 O9 2.149(5) . ?
Mn2 O6 2.203(4) . ?
Mn2 O1 2.261(5) 2_666 ?
Mn2 N1 2.316(5) . ?
Mn2 O2 2.325(4) 2_666 ?
N1 C13 1.321(8) . ?
N1 C12 1.336(7) . ?
O1 C1 1.249(8) . ?
O2 C1 1.252(7) . ?
O3 C8 1.254(7) . ?
O4 C8 1.263(7) . ?
O5 C14 1.242(7) . ?
O6 C14 1.264(7) . ?
O10 O10 1.452(17) 2_565 ?
C1 C2 1.503(8) . ?
C2 C7 1.383(8) . ?
C2 C3 1.397(8) . ?
C3 C4 1.394(8) . ?
C4 C5 1.373(8) . ?
C4 C8 1.502(7) . ?
C5 C6 1.397(8) . ?
C6 C7 1.398(8) . ?
C6 C9 1.491(8) . ?
C9 C13 1.397(8) . ?
C9 C10 1.398(8) . ?
C10 C11 1.377(8) . ?
C11 C12 1.384(8) . ?
C12 C14 1.513(8) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O12 H12D O11 0.85 2.03 2.880(19) 178.2 2_666 yes
O12 H12C O1 0.85 2.34 3.051(16) 141.7 . yes
O11 H11A O1 0.85 2.38 3.175(14) 156.9 . yes
O11 H11C O4 0.85 2.17 2.987(12) 160.6 1_445 yes
O8 H8D O6 0.85 2.09 2.778(6) 137.3 . yes
O8 H8B O2 0.85 2.20 2.901(6) 139.5 1_454 yes
O7 H7C O2 0.85 2.08 2.839(6) 149.2 1_554 yes
O7 H7B O3 0.85 1.93 2.734(6) 156.5 2_776 yes
O10 H10C O6 0.85 2.58 3.276(10) 140.2 2_565 yes
O10 H10C O3 0.85 2.33 2.773(10) 112.8 1_444 yes
O10 H10B O3 0.85 2.29 2.995(10) 141.0 2_676 yes
O9 H9D O3 0.85 2.34 2.833(7) 117.2 2_776 yes
O9 H9B O4 0.85 2.60 3.352(7) 148.9 2_776 yes
O9 H9B O4 0.85 2.60 3.352(7) 148.9 2_776 yes
O9 H9D O3 0.85 2.34 2.833(7) 117.2 2_776 yes
O10 H10B O3 0.85 2.29 2.995(10) 141.0 2_676 yes
O10 H10C O3 0.85 2.33 2.773(10) 112.8 1_444 yes
O10 H10C O6 0.85 2.58 3.276(10) 140.2 2_565 yes
O7 H7B O3 0.85 1.93 2.734(6) 156.5 2_776 yes
O7 H7C O2 0.85 2.08 2.839(6) 149.2 1_554 yes
O8 H8B O2 0.85 2.20 2.901(6) 139.5 1_454 yes
O8 H8D O6 0.85 2.09 2.778(6) 137.3 . yes
O11 H11C O4 0.85 2.17 2.987(12) 160.6 1_445 yes
O11 H11A O1 0.85 2.38 3.175(14) 156.9 . yes
O12 H12C O1 0.85 2.34 3.051(16) 141.7 . yes
O12 H12D O11 0.85 2.03 2.880(19) 178.2 2_666 yes
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
_geom_torsion_publ_flag
Mn2 O1 C1 O2 0.7(7) 2_666 . . . ?
Mn2 O1 C1 C2 -177.8(5) 2_666 . . . ?
Mn2 O2 C1 O1 -0.7(7) 2_666 . . . ?
Mn2 O2 C1 C2 177.8(5) 2_666 . . . ?
O1 C1 C2 C7 -4.4(9) . . . . ?
O2 C1 C2 C7 177.0(6) . . . . ?
O1 C1 C2 C3 172.4(6) . . . . ?
O2 C1 C2 C3 -6.2(9) . . . . ?
C7 C2 C3 C4 1.8(9) . . . . ?
C1 C2 C3 C4 -175.0(5) . . . . ?
C2 C3 C4 C5 -1.5(9) . . . . ?
C2 C3 C4 C8 176.0(5) . . . . ?
C3 C4 C5 C6 -1.0(9) . . . . ?
C8 C4 C5 C6 -178.5(5) . . . . ?
C4 C5 C6 C7 3.1(9) . . . . ?
C4 C5 C6 C9 -177.8(5) . . . . ?
C3 C2 C7 C6 0.3(9) . . . . ?
C1 C2 C7 C6 177.1(5) . . . . ?
C5 C6 C7 C2 -2.7(9) . . . . ?
C9 C6 C7 C2 178.1(5) . . . . ?
Mn2 O4 C8 O3 -96.6(6) 2_676 . . . ?
Mn2 O4 C8 C4 84.4(6) 2_676 . . . ?
C5 C4 C8 O3 -155.0(6) . . . . ?
C3 C4 C8 O3 27.5(8) . . . . ?
C5 C4 C8 O4 24.1(8) . . . . ?
C3 C4 C8 O4 -153.5(6) . . . . ?
C5 C6 C9 C13 -172.8(6) . . . . ?
C7 C6 C9 C13 6.4(9) . . . . ?
C5 C6 C9 C10 5.8(8) . . . . ?
C7 C6 C9 C10 -175.0(6) . . . . ?
C13 C9 C10 C11 0.2(9) . . . . ?
C6 C9 C10 C11 -178.5(5) . . . . ?
C9 C10 C11 C12 0.2(9) . . . . ?
C13 N1 C12 C11 0.0(9) . . . . ?
Mn2 N1 C12 C11 172.6(4) . . . . ?
C13 N1 C12 C14 -178.4(5) . . . . ?
Mn2 N1 C12 C14 -5.8(6) . . . . ?
C10 C11 C12 N1 -0.4(9) . . . . ?
C10 C11 C12 C14 177.9(5) . . . . ?
C12 N1 C13 C9 0.6(9) . . . . ?
Mn2 N1 C13 C9 -170.9(4) . . . . ?
C10 C9 C13 N1 -0.7(9) . . . . ?
C6 C9 C13 N1 178.0(5) . . . . ?
Mn1 O5 C14 O6 -13.1(9) . . . . ?
Mn1 O5 C14 C12 166.9(4) . . . . ?
Mn2 O6 C14 O5 178.1(4) . . . . ?
Mn2 O6 C14 C12 -2.0(7) . . . . ?
N1 C12 C14 O5 -174.7(5) . . . . ?
C11 C12 C14 O5 7.0(8) . . . . ?
N1 C12 C14 O6 5.4(8) . . . . ?
C11 C12 C14 O6 -173.0(5) . . . . ?
