Charge, adsorption, water stability and bandgap tuning of an anionic Cd(ii) porphyrinic metal-organic framework.
Li, Qi; Luo, Yanping; Ding, Yue; Wang, Yina; Wang, Yuxin; Du, Hongbin; Yuan, Rongxin; Bao, Jianchun; Fang, Min; Wu, Yong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8678–8692; doi:10.1039/c9dt00478e

data_7700026
_publ_section_title
;
 Charge, adsorption, water stability and bandgap tuning of an anionic
 Cd(ii) porphyrinic metal-organic framework.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8678
_journal_page_last               8692
_journal_paper_doi               10.1039/c9dt00478e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '0.5(C192 H104 Cd6.54 N16 O32)'
_chemical_formula_sum            'C113.76 H102.04 Cd3.31 N14.38 O23'
_chemical_formula_weight         2390.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-26 deposited with the CCDC.    2019-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.216(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0923(16)
_cell_length_b                   26.431(6)
_cell_length_c                   30.165(8)
_cell_measurement_reflns_used    5610
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.92
_cell_measurement_theta_min      2.55
_cell_volume                     5631(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.1403
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            57091
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.139
_diffrn_reflns_theta_min         1.683
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0697 before and 0.0597 after correction. The Ratio of minimum to maximum transmission is 0.9095. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.012
_platon_squeeze_details
;
TITL mo_3_collect_0ma_a.res in C2/c
CELL    7.0923   26.4310   30.1650     90.00     95.22     90.00
SPGR C2/c
C101 0.280 0.450 0.949 !       2.08 eA-3
C102 1.000 0.125 0.755 !       2.04 eA-3
Q103 0.909 0.383 0.740 !       2.00 eA-3
C104 0.401 0.266 0.250 !       1.80 eA-3
Q105 0.910 0.018 0.775 !       1.74 eA-3
C106 0.501 0.289 0.250 !       1.66 eA-3
C107 0.850 0.201 0.744 !       1.62 eA-3
C108 1.000 0.328 0.255 !       1.61 eA-3
C109 0.435 0.320 0.246 !       1.59 eA-3
Q110 0.426 0.119 0.264 !       1.55 eA-3
C111 0.569 0.386 0.229 !       1.52 eA-3
C112 0.685 0.086 0.431 !       1.51 eA-3
Q113 0.970 0.218 0.267 !       1.46 eA-3
C114 0.111 0.418 0.908 !       1.44 eA-3
C115 0.650 0.359 0.251 !       1.42 eA-3
C116 0.850 0.141 0.749 !       1.42 eA-3
C117 0.810 0.033 0.416 !       1.41 eA-3
C118 0.223 0.298 0.250 !       1.40 eA-3
C119 0.875 0.350 0.249 !       1.38 eA-3
C120 1.000 0.289 0.250 !       1.36 eA-3
Q121 0.500 0.492 0.745 !       1.35 eA-3
C122 0.076 0.431 0.921 !       1.34 eA-3
C123 0.784 0.173 0.745 !       1.31 eA-3
C124 0.889 0.048 0.422 !       1.31 eA-3
C125 0.434 0.383 0.231 !       1.24 eA-3
Q126 0.442 0.068 0.274 !       1.23 eA-3
C127 0.253 0.358 0.256 !       1.21 eA-3
C128 0.889 0.065 0.468 !       1.18 eA-3
C129 0.599 0.180 0.758 !       1.17 eA-3
Q130 0.999 0.023 0.748 !       1.15 eA-3
C131 0.248 0.370 0.232 !       1.14 eA-3
Q132 0.553 0.500 0.291 !       1.14 eA-3
C133 0.687 0.421 0.519 !       1.11 eA-3
C134 0.627 0.342 0.226 !       1.10 eA-3
Q135 1.000 0.484 0.753 !       1.08 eA-3
C136 1.001 0.258 0.247 !       1.07 eA-3
C137 0.658 0.494 0.562 !       1.04 eA-3
Q138 0.500 0.445 0.253 !       1.04 eA-3
C139 0.092 0.012 0.093 !       1.02 eA-3
Q140 0.411 0.047 0.240 !       1.01 eA-3
C141 0.464 0.015 0.033 !       1.01 eA-3
C142 0.994 0.008 0.063 !       1.00 eA-3
C143 0.301 0.482 0.969 !       0.99 eA-3
Q144 0.991 0.073 0.412 !       0.99 eA-3
C145 0.280 0.257 0.252 !       0.98 eA-3
C146 0.987 0.367 0.264 !       0.97 eA-3
C147 0.906 0.492 0.010 !       0.97 eA-3
C148 0.781 0.242 0.748 !       0.97 eA-3
C149 0.491 0.501 0.530 !       0.96 eA-3
Q150 0.999 0.422 0.247 !       0.96 eA-3
C151 0.619 0.101 0.443 !       0.95 eA-3
C152 0.481 0.451 0.550 !       0.95 eA-3
C153 0.748 0.117 0.444 !       0.93 eA-3
C154 0.940 0.267 0.219 !       0.93 eA-3
C155 0.852 0.284 0.232 !       0.92 eA-3
C156 0.872 0.091 0.430 !       0.92 eA-3
C157 0.649 0.242 0.742 !       0.92 eA-3
C158 0.469 0.018 0.493 !       0.92 eA-3
C159 0.349 0.227 0.789 !       0.92 eA-3
Q160 0.026 0.068 0.273 !       0.92 eA-3
C161 0.500 0.500 0.000 !       0.91 eA-3
C162 0.267 0.092 0.031 !       0.89 eA-3
Q163 0.247 0.244 0.210 !       0.88 eA-3
Q164 0.138 0.226 0.219 !       0.88 eA-3
C165 0.062 0.022 0.547 !       0.87 eA-3
C166 0.296 0.452 0.990 !       0.87 eA-3
Q167 0.321 0.132 0.272 !       0.87 eA-3
Q168 0.500 0.180 0.251 !       0.86 eA-3
C169 0.907 0.014 0.016 !       0.86 eA-3
Q170 0.595 0.059 0.393 !       0.83 eA-3
Q171 0.626 0.120 0.414 !       0.83 eA-3
Q172 0.841 0.064 0.235 !       0.80 eA-3
Q173 0.689 0.259 0.312 !       0.80 eA-3
Q174 0.803 0.048 0.087 !       0.80 eA-3
C175 0.088 0.491 0.015 !       0.80 eA-3
Q176 0.428 0.327 0.205 !       0.79 eA-3
Q177 0.282 0.437 0.272 !       0.79 eA-3
Q178 0.532 0.317 0.210 !       0.79 eA-3
C179 0.302 0.076 0.006 !       0.78 eA-3
Q180 0.379 0.068 0.432 !       0.78 eA-3
C181 0.095 0.025 0.452 !       0.78 eA-3
Q182 0.375 0.421 0.227 !       0.78 eA-3
Q183 0.504 0.023 0.762 !       0.78 eA-3
Q184 0.509 0.081 0.444 !       0.77 eA-3
C185 0.356 0.257 0.280 !       0.77 eA-3
Q186 0.037 0.239 0.212 !       0.77 eA-3
C187 0.820 0.452 0.493 !       0.76 eA-3
C188 0.679 0.382 0.525 !       0.76 eA-3
Q189 0.970 0.131 0.800 !       0.76 eA-3
C190 0.235 0.399 0.255 !       0.76 eA-3
Q191 0.756 0.008 0.392 !       0.75 eA-3
Q192 0.943 0.151 0.257 !       0.75 eA-3
Q193 0.332 0.283 0.164 !       0.75 eA-3
Q194 0.978 0.173 0.219 !       0.74 eA-3
C195 0.058 0.461 0.541 !       0.74 eA-3
Q196 0.069 0.014 0.408 !       0.73 eA-3
Q197 0.933 0.202 0.289 !       0.73 eA-3
Q198 0.346 0.360 0.924 !       0.73 eA-3
Q199 0.901 0.024 0.557 !       0.72 eA-3
;
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6182
_refine_ls_number_restraints     806
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1720
_refine_ls_R_factor_gt           0.0923
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+52.8405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3224
_reflns_number_total             6182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00478e2.cif
_cod_data_source_block           mo_3_collect_0ma_sq
_cod_depositor_comments
'Adding full bibliography for 7700026--7700027.cif.'
_cod_database_code               7700026
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.964
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C18A-C17A
 1.5 with sigma of 0.02
 C24A-C21A
 1.5 with sigma of 0.02
 O3A-C24A
 1.24 with sigma of 0.02
 O4A-C24A
 1.24 with sigma of 0.02
 O3B-C24B
 1.24 with sigma of 0.02
 O4B-C24B
 1.24 with sigma of 0.02
3. Rigid bond restraints
 C12, C10, C11, C9, C8, C1, C16B, C19B, C15B, C23B, C21B, C13B, C18B, C14B,
 C24B, C22B, C20B, C17B, C13A, C21A, C14A, C19A, C22A, C15A, C17A, C23A, C18A,
 C16A, C24A, C20A, C3B, C2B, C7B, C6B, C5B, C4B, C5A, C6A, C7A, C2A, C3A, C4A,
 N1, N2B, N2A, O2, O1, O4B, O3B, O4A, O3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C12 \\sim C10 \\sim C11 \\sim C9 \\sim C8 \\sim C1 \\sim C16B \\sim C19B \\sim
C15B \\sim C23B \\sim C21B \\sim C13B \\sim C18B \\sim C14B \\sim C24B \\sim
C22B \\sim C20B \\sim C17B \\sim C13A \\sim C21A \\sim C14A \\sim C19A \\sim
C22A \\sim C15A \\sim C17A \\sim C23A \\sim C18A \\sim C16A \\sim C24A \\sim
C20A \\sim C3B \\sim C2B \\sim C7B \\sim C6B \\sim C5B \\sim C4B \\sim C5A
\\sim C6A \\sim C7A \\sim C2A \\sim C3A \\sim C4A \\sim N1 \\sim N2B \\sim N2A
\\sim O2 \\sim O1 \\sim O4B \\sim O3B \\sim O4A \\sim O3A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=
 Sof(C4A)=Sof(H4A)=1-FVAR(1)
 Sof(C3B)=Sof(H3B)=Sof(C2B)=Sof(C7B)=Sof(H7B)=Sof(C6B)=Sof(H6B)=Sof(C5B)=
 Sof(C4B)=Sof(H4B)=FVAR(1)
 Sof(O4B)=Sof(O3B)=Sof(N2B)=Sof(C16B)=Sof(C19B)=Sof(H19B)=Sof(C15B)=Sof(H15B)=
 Sof(C23B)=Sof(H23B)=Sof(C21B)=Sof(C13B)=Sof(C18B)=Sof(C14B)=Sof(H14B)=
 Sof(C24B)=Sof(C22B)=Sof(H22B)=Sof(C20B)=Sof(H20B)=Sof(C17B)=1-FVAR(2)
 Sof(Cd2)=Sof(O4A)=Sof(O3A)=Sof(N2A)=Sof(C13A)=Sof(C21A)=Sof(C14A)=Sof(H14A)=
 Sof(C19A)=Sof(H19A)=Sof(C22A)=Sof(H22A)=Sof(C15A)=Sof(H15A)=Sof(C17A)=
 Sof(C23A)=Sof(H23A)=Sof(C18A)=Sof(C16A)=Sof(C24A)=Sof(C20A)=Sof(H20A)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C10(H10), C11(H11), C19B(H19B), C15B(H15B), C23B(H23B), C14B(H14B),
 C22B(H22B), C20B(H20B), C14A(H14A), C19A(H19A), C22A(H22A), C15A(H15A),
 C23A(H23A), C20A(H20A), C3B(H3B), C7B(H7B), C6B(H6B), C4B(H4B), C6A(H6A),
 C7A(H7A), C3A(H3A), C4A(H4A)
6.b Fitted hexagon refined as free rotating group:
 C3B(C2B,C7B,C6B,C5B,C4B), C5A(C6A,C7A,C2A,C3A,C4A)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'