Four new metal-organic frameworks based on diverse secondary building units: sensing and magnetic properties.
Yan, Yang-Tian; Zhang, Wen-Yan; Zhang, Fang; Cao, Feng; Yang, Rui-Feng; Wang, Yao-Yu; Hou, Lei; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1682–1692; doi:10.1039/c7dt04696k

data_7045168
_publ_section_title
;
 Four new metal-organic frameworks based on diverse secondary building
 units: sensing and magnetic properties.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1682
_journal_page_last               1692
_journal_paper_doi               10.1039/c7dt04696k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C23 H11 O11 Zn2, C2 H8 N'
_chemical_formula_sum            'C25 H19 N O11 Zn2'
_chemical_formula_weight         640.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-12-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                65.009(7)
_cell_angle_beta                 79.056(7)
_cell_angle_gamma                79.551(7)
_cell_formula_units_Z            2
_cell_length_a                   12.252(5)
_cell_length_b                   12.820(5)
_cell_length_c                   13.635(6)
_cell_measurement_reflns_used    4146
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.253
_cell_measurement_theta_min      2.526
_cell_volume                     1893.5(14)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10198
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         6.822
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0662 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.8001.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_platon_squeeze_details
;
TITL 1_sq      P -1         R = 0.11
CELL   12.2520   12.8200   13.6350     65.01     79.06     79.55
SPGR P-1
C101 0.466 0.324 0.348 !       3.83 eA-3
Q102 0.607 0.533 0.372 !       3.71 eA-3
C103 0.144 0.879 0.411 !       3.57 eA-3
C104 0.415 0.669 0.328 !       3.57 eA-3
C105 0.486 0.671 0.406 !       3.52 eA-3
C106 0.160 0.963 0.217 !       3.40 eA-3
C107 0.100 0.967 0.325 !       3.37 eA-3
C108 0.383 0.421 0.278 !       3.18 eA-3
C109 0.467 0.318 0.438 !       3.14 eA-3
C110 0.285 0.817 0.317 !       2.95 eA-3
C111 0.455 0.753 0.454 !       2.94 eA-3
Q112 0.667 0.625 0.013 !       2.94 eA-3
C113 0.525 0.237 0.506 !       2.79 eA-3
C114 0.578 0.590 0.425 !       2.50 eA-3
C115 0.551 0.284 0.283 !       2.42 eA-3
C116 0.192 0.894 0.313 !       2.38 eA-3
Q117 0.690 0.471 0.377 !       2.29 eA-3
Q118 0.097 0.372 0.012 !       2.15 eA-3
C119 0.984 0.424 0.113 !       2.13 eA-3
C120 0.019 0.402 0.185 !       2.04 eA-3
C121 0.328 0.746 0.406 !       2.03 eA-3
C122 0.401 0.784 0.308 !       1.99 eA-3
C123 0.996 0.323 0.232 !       1.99 eA-3
Q124 0.671 0.476 0.298 !       1.93 eA-3
Q125 0.748 0.520 0.328 !       1.91 eA-3
Q126 0.469 0.134 0.112 !       1.87 eA-3
C127 0.965 0.386 0.041 !       1.83 eA-3
C128 0.186 0.830 0.474 !       1.79 eA-3
C129 0.953 0.543 0.063 !       1.67 eA-3
Q130 0.437 0.084 0.079 !       1.56 eA-3
Q131 0.934 0.499 0.472 !       1.55 eA-3
C132 0.535 0.294 0.368 !       1.54 eA-3
C133 0.971 0.371 0.140 !       1.53 eA-3
Q134 0.455 0.058 0.198 !       1.50 eA-3
C135 0.952 0.365 0.107 !       1.47 eA-3
C136 0.437 0.394 0.215 !       1.43 eA-3
C137 0.391 0.448 0.351 !       1.42 eA-3
C138 0.027 0.494 0.093 !       1.35 eA-3
C139 1.001 0.220 0.220 !       1.35 eA-3
C140 0.530 0.466 0.393 !       1.33 eA-3
C141 0.061 0.140 0.233 !       1.31 eA-3
Q142 0.621 0.609 0.487 !       1.30 eA-3
C143 0.855 0.203 0.268 !       1.30 eA-3
C144 0.416 0.355 0.482 !       1.29 eA-3
C145 0.030 0.553 0.009 !       1.28 eA-3
C146 0.935 0.304 0.184 !       1.26 eA-3
C147 0.799 0.274 0.305 !       1.25 eA-3
C148 0.980 0.197 0.280 !       1.24 eA-3
Q149 0.896 0.466 0.430 !       1.23 eA-3
C150 0.913 0.321 0.097 !       1.22 eA-3
Q151 0.432 0.996 0.280 !       1.21 eA-3
Q152 0.454 0.823 0.043 !       1.19 eA-3
Q153 0.500 1.000 0.000 !       1.19 eA-3
Q154 0.512 0.939 0.058 !       1.19 eA-3
Q155 0.876 0.406 0.486 !       1.17 eA-3
C156 0.033 0.071 0.301 !       1.16 eA-3
C157 0.487 0.522 0.373 !       1.16 eA-3
C158 0.513 0.360 0.237 !       1.16 eA-3
C159 0.059 0.262 0.225 !       1.16 eA-3
C160 0.943 0.062 0.405 !       1.15 eA-3
C161 1.002 0.030 0.344 !       1.14 eA-3
C162 0.975 0.082 0.422 !       1.12 eA-3
Q163 0.112 0.627 0.402 !       1.12 eA-3
C164 0.707 0.249 0.270 !       1.12 eA-3
Q165 0.968 0.455 0.245 !       1.10 eA-3
Q166 0.465 0.765 0.297 !       1.10 eA-3
Q167 0.143 0.668 0.378 !       1.10 eA-3
Q168 0.331 0.301 0.471 !       1.09 eA-3
C169 0.098 0.369 0.112 !       1.08 eA-3
C170 0.606 0.208 0.334 !       1.08 eA-3
Q171 0.752 0.608 0.039 !       1.07 eA-3
Q172 0.327 0.908 0.227 !       1.07 eA-3
Q173 0.861 0.222 0.467 !       1.05 eA-3
Q174 0.575 0.927 0.096 !       1.05 eA-3
Q175 0.311 0.089 0.416 !       1.05 eA-3
Q176 0.108 0.554 0.442 !       1.05 eA-3
Q177 0.985 0.345 0.377 !       1.05 eA-3
Q178 0.705 0.217 0.068 !       1.05 eA-3
Q179 0.099 0.563 0.482 !       1.04 eA-3
Q180 0.659 0.571 0.081 !       1.03 eA-3
C181 0.834 0.314 0.135 !       1.01 eA-3
Q182 0.358 0.083 0.155 !       1.00 eA-3
Q183 0.891 0.831 0.222 !       0.99 eA-3
C184 0.909 0.099 0.470 !       0.99 eA-3
Q185 0.908 0.811 0.262 !       0.98 eA-3
C186 0.061 0.251 0.167 !       0.98 eA-3
Q187 0.135 0.335 0.156 !       0.97 eA-3
Q188 0.514 0.578 0.062 !       0.97 eA-3
Q189 0.715 0.883 0.168 !       0.96 eA-3
C190 0.123 0.897 0.484 !       0.96 eA-3
C191 0.541 0.329 0.465 !       0.96 eA-3
Q192 0.278 0.107 0.346 !       0.95 eA-3
Q193 0.189 0.083 0.297 !       0.95 eA-3
C194 0.886 0.175 0.453 !       0.95 eA-3
Q195 0.473 0.703 0.060 !       0.94 eA-3
C196 0.920 0.061 0.328 !       0.94 eA-3
Q197 0.732 0.455 0.431 !       0.93 eA-3
Q198 0.441 0.295 0.256 !       0.93 eA-3
Q199 0.788 0.220 0.407 !       0.93 eA-3

;
_refine_diff_density_max         1.629
_refine_diff_density_min         -1.560
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7377
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0791
_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          0.2428
_refine_ls_wR_factor_ref         0.3037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5713
_reflns_number_total             7377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04696k1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045167--7045170.cif.'
_cod_original_cell_volume        1893.6(14)
_cod_database_code               7045168
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C5)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 N1, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 O11(H11A,H11B)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C10(H10), C12(H12), C14(H14), C17(H17), C18(H18),
 C20(H20)
4.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_fab_checksum              49078
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'