An anionic manganese(ii) metal‒organic framework for uranyl adsorption
Zhang, Tao; Ling, Bo-Kai; Hu, Yue-Qiao; Han, Tian; Zheng, Yan-Zhen; CrystEngComm 21 (2019) 3901–; doi:10.1039/C9CE00603F

data_7232869
_publ_section_title
;
 An anionic manganese(ii) metal--organic framework for uranyl adsorption
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3901
_journal_paper_doi               10.1039/C9CE00603F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C21 H3 Mn5 N6 O24'
_chemical_formula_sum            'C21 H3 Mn5 N6 O24'
_chemical_formula_weight         997.99
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_symmetry_space_group_name_Hall  'I -4 -2c'
_symmetry_space_group_name_H-M   'I -4 c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-11 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.343(7)
_cell_length_b                   26.343(7)
_cell_length_c                   37.301(11)
_cell_measurement_reflns_used    9663
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.890
_cell_measurement_theta_min      1.092
_cell_volume                     25885(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omiga scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            85188
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.891
_diffrn_reflns_theta_max         24.890
_diffrn_reflns_theta_min         1.092
_exptl_absorpt_coefficient_mu    1.004
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_description       cubic
_exptl_crystal_F_000             7808
_platon_squeeze_details
;
TITL 1 in I-4c2
CELL   26.3430   26.3430   37.3010     90.00     90.00     90.00
SPGR I-4c2
C101 0.850 0.409 0.350 !       8.31 eA-3
C102 0.264 0.242 0.189 !       7.55 eA-3
C103 0.267 0.574 0.485 !       7.40 eA-3
C104 0.345 0.180 0.385 !       6.79 eA-3
C105 0.852 0.650 0.342 !       6.22 eA-3
C106 0.394 0.798 0.365 !       5.60 eA-3
C107 0.227 0.929 0.062 !       5.45 eA-3
Q108 0.991 0.364 0.351 !       5.12 eA-3
C109 0.451 0.197 0.384 !       4.76 eA-3
C110 0.892 0.250 0.232 !       4.47 eA-3
Q111 0.153 0.230 0.149 !       4.47 eA-3
Q112 0.087 0.699 0.290 !       4.36 eA-3
C113 0.593 0.051 0.390 !       4.33 eA-3
C114 0.984 0.212 0.484 !       4.27 eA-3
C115 0.208 0.144 0.182 !       4.23 eA-3
C116 0.089 0.685 0.312 !       4.23 eA-3
C117 0.564 0.976 0.352 !       4.23 eA-3
C118 0.338 0.966 0.353 !       4.08 eA-3
Q119 0.453 0.528 0.405 !       3.97 eA-3
C120 0.079 0.042 0.493 !       3.95 eA-3
C121 0.189 0.312 0.217 !       3.90 eA-3
C122 0.318 0.468 0.002 !       3.84 eA-3
C123 0.262 0.772 0.189 !       3.84 eA-3
C124 0.031 0.787 0.055 !       3.77 eA-3
C125 0.069 0.932 0.072 !       3.76 eA-3
C126 0.500 0.498 0.399 !       3.76 eA-3
C127 0.158 0.862 0.241 !       3.69 eA-3
C128 0.038 0.713 0.070 !       3.68 eA-3
Q129 0.345 0.191 0.171 !       3.67 eA-3
C130 0.951 0.306 0.078 !       3.67 eA-3
C131 0.295 0.076 0.109 !       3.63 eA-3
C132 0.189 0.288 0.278 !       3.58 eA-3
C133 0.189 0.709 0.784 !       3.54 eA-3
C134 0.500 1.001 0.336 !       3.54 eA-3
C135 0.430 0.791 0.090 !       3.53 eA-3
C136 0.268 0.045 0.055 !       3.48 eA-3
C137 0.282 0.857 0.009 !       3.47 eA-3
C138 0.547 0.767 0.947 !       3.47 eA-3
Q139 0.119 0.670 0.162 !       3.41 eA-3
C140 0.183 0.305 0.250 !       3.34 eA-3
C141 0.563 0.054 0.365 !       3.33 eA-3
C142 0.015 0.046 0.027 !       3.32 eA-3
Q143 0.788 0.103 0.006 !       3.29 eA-3
C144 0.750 0.614 0.235 !       3.25 eA-3
Q145 0.563 0.329 0.939 !       3.20 eA-3
Q146 0.063 0.829 0.439 !       3.20 eA-3
C147 0.259 0.466 0.429 !       3.14 eA-3
C148 0.773 0.485 0.010 !       3.12 eA-3
Q149 0.076 0.271 0.078 !       3.11 eA-3
C150 0.484 0.856 0.382 !       3.11 eA-3
C151 0.885 0.323 0.375 !       3.08 eA-3
C152 0.944 0.068 0.462 !       3.08 eA-3
C153 0.600 0.563 0.433 !       3.05 eA-3
C154 0.906 0.341 0.398 !       3.02 eA-3
C155 0.555 0.928 0.439 !       3.01 eA-3
C156 0.658 0.882 0.146 !       3.01 eA-3
Q157 0.834 0.337 0.022 !       2.99 eA-3
C158 0.935 0.556 0.447 !       2.98 eA-3
C159 0.532 0.208 0.092 !       2.97 eA-3
C160 0.038 0.277 0.921 !       2.94 eA-3
C161 0.538 0.777 0.421 !       2.94 eA-3
C162 0.295 0.472 0.460 !       2.94 eA-3
Q163 0.532 0.821 0.354 !       2.93 eA-3
Q164 0.141 0.328 0.468 !       2.92 eA-3
C165 0.486 0.145 0.383 !       2.91 eA-3
C166 0.334 0.090 0.022 !       2.90 eA-3
C167 0.875 0.313 0.454 !       2.90 eA-3
C168 0.196 0.827 0.226 !       2.88 eA-3
C169 0.937 0.464 0.403 !       2.87 eA-3
C170 0.119 0.648 0.432 !       2.87 eA-3
C171 0.583 0.785 0.421 !       2.85 eA-3
C172 0.858 0.511 0.485 !       2.83 eA-3
Q173 0.304 0.997 0.123 !       2.80 eA-3
Q174 0.723 0.507 0.431 !       2.75 eA-3
C175 0.092 0.401 0.014 !       2.74 eA-3
Q176 0.213 0.702 0.179 !       2.74 eA-3
Q177 0.339 0.835 0.094 !       2.73 eA-3
C178 0.968 0.578 0.375 !       2.73 eA-3
C179 0.169 0.946 0.430 !       2.71 eA-3
C180 0.189 0.548 0.383 !       2.70 eA-3
Q181 0.946 0.245 0.226 !       2.70 eA-3
Q182 0.578 0.183 0.569 !       2.70 eA-3
Q183 0.078 0.683 0.069 !       2.70 eA-3
C184 0.390 0.842 0.058 !       2.70 eA-3
C185 0.765 0.641 0.221 !       2.70 eA-3
C186 0.337 0.689 0.288 !       2.69 eA-3
Q187 0.087 0.682 0.181 !       2.69 eA-3
C188 0.784 0.577 0.009 !       2.67 eA-3
C189 0.320 0.684 0.344 !       2.66 eA-3
Q190 0.726 0.213 0.670 !       2.66 eA-3
Q191 0.501 0.848 0.161 !       2.65 eA-3
Q192 0.586 0.110 0.155 !       2.64 eA-3
C193 0.977 0.716 0.016 !       2.64 eA-3
C194 0.108 0.300 0.065 !       2.63 eA-3
Q195 0.987 0.052 0.116 !       2.63 eA-3
C196 0.500 0.999 0.461 !       2.61 eA-3
C197 0.454 0.863 0.407 !       2.60 eA-3
C198 0.015 0.551 0.439 !       2.60 eA-3
C199 0.155 0.157 0.249 !       2.60 eA-3
;
_refine_diff_density_max         1.000
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         11061
_refine_ls_number_restraints     430
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0926
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2405
_refine_ls_wR_factor_ref         0.2546
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                9401
_reflns_number_total             11061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00603f2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments          'Adding full bibliography for 7232869.cif.'
_cod_original_cell_volume        25885(16)
_cod_database_code               7232869
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.63(5)
 0.37(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C20-C19
 2.2 with sigma of 0.02
4. Rigid bond restraints
 C12, C18, C20, C11, C21, C3, C10, C13, C4, C15, C19, C8, C16, C5, C14, C2, C6,
  C17, C1, C7, C9, N3, N1, N2, N6, N5, N4, O20, O6, O23, O17, O4, O1, O21, O19,
 O24, O7, O10, O16, O13, O2, O8, O3, O12, O18, O15, O11, O22, O5, O14, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C12 \\sim C18 \\sim C20 \\sim C11 \\sim C21 \\sim C3 \\sim C10 \\sim C13 \\sim
C4 \\sim C15 \\sim C19 \\sim C8 \\sim C16 \\sim C5 \\sim C14 \\sim C2 \\sim C6
\\sim C17 \\sim C1 \\sim C7 \\sim C9 \\sim N3 \\sim N1 \\sim N2 \\sim N6 \\sim
N5 \\sim N4 \\sim O20 \\sim O6 \\sim O23 \\sim O17 \\sim O4 \\sim O1 \\sim O21
\\sim O19 \\sim O24 \\sim O7 \\sim O10 \\sim O16 \\sim O13 \\sim O2 \\sim O8
\\sim O3 \\sim O12 \\sim O18 \\sim O15 \\sim O11 \\sim O22 \\sim O5 \\sim O14
\\sim O9: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C19(H19), C5(H5)
;
_shelx_res_checksum              49490
_shelx_fab_checksum              14858
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20
_platon_1_sq_details
;
Disordered volatile and ionic guests per formula unit were removed by SQUEEZE.
The values were calculated
based on elemental analysis and TGA data.
Guest = 5K+,7CH3CN and 8H2O
;