A covalent deprotection strategy for assembling supramolecular coordination polymers from metal-organic cages.
Schneider, Matthew L.; Linder-Patton, Oliver M; Bloch, Witold M.; Chemical communications (Cambridge, England) 56 (2020) 12969–12972; doi:10.1039/d0cc05349j

data_7127302
_publ_section_title
;
 A covalent deprotection strategy for assembling supramolecular
 coordination polymers from metal-organic cages.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12969
_journal_page_last               12972
_journal_paper_doi               10.1039/d0cc05349j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C19 H13 N3 O2 Pt'
_chemical_formula_sum            'C19 H13 N3 O2 Pt'
_chemical_formula_weight         510.41
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-14 deposited with the CCDC.	2020-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   30.402(2)
_cell_length_b                   30.402(2)
_cell_length_c                   10.0404(8)
_cell_measurement_reflns_used    1430
_cell_measurement_temperature    150
_cell_measurement_theta_max      62.5290
_cell_measurement_theta_min      2.8500
_cell_volume                     8036.9(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  24.00   0.50    2.25    --  -46.37  62.00 -36.00  174
  2  \w    -47.00 -11.00   0.50    7.18    --  -84.50  37.00-180.00   72
  3  \w    -81.00 -56.00   0.50    7.18    --  -84.50  62.00 -36.00   50
  4  \w   -113.00 -59.00   0.50    2.25    --  -46.37 -62.00-173.00  108
  5  \w   -136.00-111.00   0.50    7.18    --  -84.50 -62.00-173.00   50
  6  \w     12.00  45.00   0.50    2.25    --   46.37 -62.00-173.00   66
  7  \w     73.00 119.00   0.50    7.18    --  108.56 -62.00-173.00   92
  8  \w     38.00  72.00   0.50    7.18    --  108.56 -62.00-173.00   68
  9  \w     42.00  69.00   0.50    7.18    --  108.56 -37.00-180.00   54
 10  \w     37.00  62.00   0.50    7.18    --  108.56 -37.00-120.00   50
 11  \w     36.00  63.00   0.50    7.18    --  108.56 -37.00-150.00   54
 12  \w     36.00  69.00   0.50    7.18    --  108.56 -37.00 -30.00   66
 13  \w     38.00  69.00   0.50    7.18    --  108.56 -37.00   0.00   62
 14  \w     39.00  68.00   0.50    7.18    --  108.56 -37.00  30.00   58
 15  \w     42.00  76.00   0.50    7.18    --  108.56 -19.00  30.00   68
 16  \w     36.00  68.00   0.50    7.18    --  108.56 -19.00   0.00   64
 17  \w     37.00  67.00   0.50    7.18    --  108.56 -37.00  60.00   60
 18  \w     66.00  93.00   0.50    7.18    --  108.56 -99.00  60.00   54
 19  \w     35.00  65.00   0.50    7.18    --  108.56 -19.00 150.00   60
 20  \w    139.00 176.00   0.50    7.18    --  108.56  62.00 -36.00   74
 21  \w     78.00 118.00   0.50    2.25    --   46.37 125.00-180.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0341254333
_diffrn_orient_matrix_UB_12      -0.0112811667
_diffrn_orient_matrix_UB_13      0.1234019333
_diffrn_orient_matrix_UB_21      -0.0452478333
_diffrn_orient_matrix_UB_22      -0.0418749667
_diffrn_orient_matrix_UB_23      -0.0776967667
_diffrn_orient_matrix_UB_31      0.0145125333
_diffrn_orient_matrix_UB_32      -0.0392733333
_diffrn_orient_matrix_UB_33      0.0476595667
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1143
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12983
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.013
_diffrn_reflns_theta_min         2.907
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45h (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       needle
_exptl_crystal_F_000             4356
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_platon_squeeze_details
;
TITL ptbimpic_para_a.res in R-3
CELL   30.4020   30.4020   10.0404     90.00     90.00    120.00
SPGR R-3
Q101 0.672 0.657 0.558 !       3.06 eA-3
C102 0.961 0.939 0.377 !       2.40 eA-3
C103 0.266 0.612 0.368 !       2.13 eA-3
C104 0.663 0.267 0.375 !       1.95 eA-3
C105 1.001 0.024 0.618 !       1.92 eA-3
Q106 0.680 0.994 0.184 !       1.86 eA-3
Q107 0.657 0.019 0.313 !       1.83 eA-3
C108 0.280 0.665 0.066 !       1.77 eA-3
C109 0.602 0.313 0.467 !       1.76 eA-3
C110 0.664 0.350 0.980 !       1.76 eA-3
C111 1.000 1.001 0.471 !       1.75 eA-3
C112 0.664 0.297 0.811 !       1.74 eA-3
C113 0.297 0.617 0.378 !       1.74 eA-3
C114 0.670 0.336 0.185 !       1.72 eA-3
Q115 0.022 0.672 0.318 !       1.69 eA-3
C116 0.243 0.602 0.292 !       1.69 eA-3
C117 0.992 0.943 0.750 !       1.68 eA-3
C118 0.008 0.971 0.091 !       1.67 eA-3
C119 0.039 0.058 0.931 !       1.67 eA-3
Q120 0.367 0.415 0.529 !       1.61 eA-3
C121 0.649 0.382 0.843 !       1.60 eA-3
C122 0.351 0.618 0.157 !       1.60 eA-3
C123 0.719 0.346 0.499 !       1.53 eA-3
C124 0.299 0.703 0.370 !       1.50 eA-3
C125 0.663 0.338 0.033 !       1.49 eA-3
C126 0.665 0.336 0.274 !       1.48 eA-3
C127 0.962 0.891 0.128 !       1.47 eA-3
C128 0.031 0.039 0.188 !       1.47 eA-3
C129 0.984 0.953-0.001 !       1.47 eA-3
C130 0.009 0.968 0.188 !       1.47 eA-3
C131 0.696 0.373 0.520 !       1.47 eA-3
C132 0.994 0.923 0.150 !       1.46 eA-3
C133 0.624 0.358 0.460 !       1.45 eA-3
C134 0.296 0.654 0.693 !       1.44 eA-3
C135 0.321 0.726 0.438 !       1.43 eA-3
C136 0.983 0.970 0.775 !       1.41 eA-3
C137 0.273 0.711 0.845 !       1.40 eA-3
C138 0.438 0.727 0.849 !       1.40 eA-3
C139 0.340 0.750 0.502 !       1.37 eA-3
Q140 0.257 0.537 0.062 !       1.37 eA-3
Q141 0.306 0.304 0.341 !       1.37 eA-3
C142 0.414 0.747 0.819 !       1.36 eA-3
Q143 1.002 0.306 0.467 !       1.34 eA-3
Q144 0.953 0.648 0.316 !       1.33 eA-3
C145 0.110 0.042 0.718 !       1.32 eA-3
C146 0.983 0.028 0.286 !       1.29 eA-3
C147 0.921 0.927 0.407 !       1.28 eA-3
C148 0.070 0.990 0.405 !       1.28 eA-3
Q149 0.018 0.882 0.407 !       1.27 eA-3
Q150 0.758 0.399 0.308 !       1.26 eA-3
C151 0.680 0.416 0.717 !       1.26 eA-3
Q152 0.475 0.774 0.937 !       1.25 eA-3
Q153 0.515 0.353 0.280 !       1.25 eA-3
C154 0.352 0.687 0.466 !       1.24 eA-3
C155 0.427 0.751 0.874 !       1.24 eA-3
C156 0.264 0.663 0.535 !       1.19 eA-3
C157 0.415 0.766 0.804 !       1.18 eA-3
C158 1.000 0.920 0.707 !       1.18 eA-3
C159 0.916 0.977 0.773 !       1.17 eA-3
C160 0.717 0.438 0.037 !       1.17 eA-3
C161 0.391 0.710 0.310 !       1.17 eA-3
Q162 0.773 0.385 0.629 !       1.16 eA-3
Q163 0.968 0.889 0.326 !       1.16 eA-3
Q164 0.389 0.096 0.470 !       1.15 eA-3
C165 0.228 0.577 0.379 !       1.14 eA-3
C166 0.254 0.632 0.875 !       1.13 eA-3
Q167 0.571 0.205 0.370 !       1.13 eA-3
C168 0.705 0.402 0.842 !       1.13 eA-3
Q169 0.148 0.397 0.219 !       1.12 eA-3
Q170 0.641 0.883 0.156 !       1.12 eA-3
Q171 0.202 0.649 0.946 !       1.11 eA-3
Q172 0.448 0.798 0.935 !       1.11 eA-3
Q173 0.633 0.805 0.130 !       1.11 eA-3
C174 0.984 0.953 0.570 !       1.09 eA-3
Q175 0.437 0.092 0.844 !       1.07 eA-3
C176 0.987 0.069 0.646 !       1.07 eA-3
Q177 0.329 0.741 0.777 !       1.05 eA-3
Q178 0.061 0.671 0.311 !       1.04 eA-3
Q179 0.939 0.329 0.689 !       1.04 eA-3
Q180 0.774 0.462 0.082 !       1.04 eA-3
Q181 0.139 0.717 0.165 !       1.03 eA-3
Q182 0.180 0.470 0.375 !       1.03 eA-3
Q183 0.711 0.029 0.254 !       1.02 eA-3
Q184 0.297 0.722 0.121 !       1.01 eA-3
Q185 0.084 0.546 0.443 !       1.01 eA-3
Q186 0.077 0.110 0.025 !       1.01 eA-3
Q187 0.609 0.539 0.193 !       0.99 eA-3
Q188 0.547 0.905 0.872 !       0.99 eA-3
Q189 0.344 0.070 0.012 !       0.99 eA-3
Q190 0.891 0.949 0.714 !       0.99 eA-3
C191 0.360 0.768-0.002 !       0.98 eA-3
Q192 0.467 0.749 0.728 !       0.97 eA-3
Q193 0.711 0.631 0.806 !       0.96 eA-3
Q194 0.111 0.476 0.088 !       0.96 eA-3
Q195 0.101 0.631 0.093 !       0.96 eA-3
Q196 0.415 0.969 0.058 !       0.95 eA-3
Q197 0.031 0.587 0.940 !       0.95 eA-3
Q198 0.272 0.750 0.383 !       0.95 eA-3
Q199 0.255 0.289 0.098 !       0.94 eA-3
;
_refine_diff_density_max         3.293
_refine_diff_density_min         -2.148
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0719
_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^)+(0.0555P)^2^+160.9555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2741
_reflns_number_total             3526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05349j2.cif
_cod_data_source_block           1P-para
_cod_depositor_comments
'Adding full bibliography for 7127299--7127303.cif.'
_cod_original_cell_volume        8037.0(13)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7127302
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H13N3O2Pt
_reflns_odcompleteness_completeness 96.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C9(H9), C12(H12), C17(H17), C14(H14), C5(H5), C16(H16), C3(H3),
 C10(H10), C2(H2A), C11(H11), C4(H4), C15(H15)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.649