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_7127301
_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, 0.67(H2 O)'
_chemical_formula_sum            'C19 H14.33 N3 O2.67 Pt'
_chemical_formula_weight         522.42
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-02
_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                   30.4714(3)
_cell_length_b                   30.4714(3)
_cell_length_c                   10.04190(10)
_cell_measurement_reflns_used    7984
_cell_measurement_temperature    150
_cell_measurement_theta_max      75.6470
_cell_measurement_theta_min      2.8780
_cell_volume                     8074.79(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     54.00 115.00   0.50    1.68    --   42.80 166.00-151.00  122
  2  \w   -131.00 -72.00   0.50    1.59    --  -84.50-123.00  68.00  118
  3  \w    -61.00 -36.00   0.50    1.59    --  -84.50  34.00-154.00   50
  4  \w    115.00 177.00   0.50    1.59    --  108.63 115.00  62.00  124
  5  \w     75.00 115.00   0.50    1.68    --   42.80 125.00-150.00   80
  6  \w     76.00 101.00   0.50    1.68    --   42.80 125.00 -90.00   50
  7  \w     31.00  63.00   0.50    1.59    --  108.63 -30.00-150.00   64
  8  \w     45.00  78.00   0.50    1.59    --  108.63 -45.00   0.00   66
  9  \w     36.00  77.00   0.50    1.59    --  108.63 -45.00 -60.00   82
 10  \w     31.00  57.00   0.50    1.59    --  108.63 -30.00 120.00   52
 11  \w     31.00  56.00   0.50    1.59    --  108.63 -34.00  48.00   50
 12  \w     39.00  65.00   0.50    1.59    --  108.63 -45.00  90.00   52
 13  \w     30.00  57.00   0.50    1.59    --  108.63 -30.00   0.00   54
 14  \w     30.00  60.00   0.50    1.59    --  108.63 -30.00-180.00   60
 15  \w     35.00  61.00   0.50    1.59    --  108.63 -30.00 -90.00   52
;
_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      0.0031769000
_diffrn_orient_matrix_UB_12      -0.0154949000
_diffrn_orient_matrix_UB_13      0.1441478000
_diffrn_orient_matrix_UB_21      -0.0346005000
_diffrn_orient_matrix_UB_22      0.0204672000
_diffrn_orient_matrix_UB_23      0.0464241000
_diffrn_orient_matrix_UB_31      -0.0468840000
_diffrn_orient_matrix_UB_32      -0.0524233000
_diffrn_orient_matrix_UB_33      -0.0245301000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8439
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.044
_diffrn_reflns_theta_max         67.044
_diffrn_reflns_theta_min         2.900
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (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    1.934
_exptl_crystal_description       block
_exptl_crystal_F_000             4476
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3188
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+29.8032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3137
_reflns_number_total             3188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05349j2.cif
_cod_data_source_block           1P
_cod_depositor_comments
'Adding full bibliography for 7127299--7127303.cif.'
_cod_original_cell_volume        8074.79(18)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7127301
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H13N3O2Pt
_shelx_estimated_absorpt_t_max   0.525
_shelx_estimated_absorpt_t_min   0.525
_reflns_odcompleteness_completeness 99.53
_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. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.04
3. Others
 Fixed Sof: O3(0.33333) O4(0.33333)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C9(H9), C2(H2A), C17(H17), C14(H14), C12(H12), C16(H16), C10(H10),
 C15(H15), C11(H11), C3(H3), C5(H5), C4(H4)
;
_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 1.447
_oxdiff_exptl_absorpt_empirical_full_min 0.750