Radical-Induced Hierarchical Self-Assembly Involving Supramolecular Coordination Complexes in Both Solution and Solid States.
Huo, Gui-Fei; Shi, Xueliang; Tu, Qian; Hu, Yi-Xiong; Wu, Gui-Yuan; Yin, Guang-Qiang; Li, Xiaopeng; Xu, Lin; Ding, Hong-Ming; Yang, Hai-Bo; Journal of the American Chemical Society 141 (2019) 16014–16023; doi:10.1021/jacs.9b08149

data_4128344
_publ_section_title
;
 Radical-Induced Hierarchical Self-Assembly Involving Supramolecular
 Coordination Complexes in Both Solution and Solid States.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16014
_journal_page_last               16023
_journal_paper_doi               10.1021/jacs.9b08149
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C19 H34 Cl3 P2 Pt'
_chemical_formula_sum            'C19 H34 Cl3 P2 Pt'
_chemical_formula_weight         625.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.1116(3)
_cell_length_b                   12.5972(2)
_cell_length_c                   14.3418(2)
_cell_measurement_reflns_used    14973
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.1270
_cell_measurement_theta_min      4.9110
_cell_volume                     4717.49(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -25.00   0.00   1.00    2.00    --    0.00 -77.00 120.00   25
  2  \w    -87.00  -2.00   1.00    2.00    --    0.00 -77.00 -60.00   85
  3  \w    -61.00  23.00   1.00    2.00    --    0.00 -57.00 150.00   84
  4  \w    -57.00  21.00   1.00    2.00    --    0.00 -57.00  30.00   78
  5  \w    -69.00 -43.00   1.00    2.00    --    0.00 -77.00 120.00   26
  6  \w     37.00  89.00   1.00    2.00    --    0.00  38.00 150.00   52
  7  \w     80.00 185.00   1.00    6.00    --   95.80  61.00 150.00  105
  8  \w     60.00 102.00   1.00    6.00    --   95.80 -82.00-120.00   42
  9  \w    117.00 144.00   1.00    6.00    --   95.80  61.00 120.00   27
 10  \w     10.00  37.00   1.00    6.00    --   95.80 -30.00  30.00   27
 11  \w     18.00 114.00   1.00    6.00    --   95.80 -30.00-180.00   96
 12  \w     87.00 162.00   1.00    6.00    --   95.80  45.00-180.00   75
 13  \w     67.00 100.00   1.00    6.00    --   95.80 -82.00 -60.00   33
 14  \w     48.00 108.00   1.00    6.00    --   95.80 -61.00  90.00   60
 15  \w     37.00 128.00   1.00    6.00    --   95.80 -82.00  90.00   91
 16  \w      7.00 101.00   1.00    6.00    --   95.80 -15.00-180.00   94
 17  \w      6.00  45.00   1.00    6.00    --   95.80 -61.00  90.00   39
 18  \w      6.00 119.00   1.00    6.00    --   95.80 -61.00 -30.00  113
 19  \w     89.00 114.00   1.00    6.00    --   95.80 -82.00  30.00   25
 20  \w     50.00 127.00   1.00    6.00    --   95.80 -82.00-180.00   77
 21  \w      7.00 117.00   1.00    6.00    --   95.80 -82.00 -30.00  110
 22  \w     76.00 101.00   1.00    6.00    --   95.80 -30.00  30.00   25
 23  \w     41.00  98.00   1.00    6.00    --   95.80 -82.00 -90.00   57
 24  \w      8.00  37.00   1.00    6.00    --   95.80 -82.00 120.00   29
 25  \w     79.00 104.00   1.00    6.00    --   95.80 -82.00 120.00   25
 26  \w     10.00  35.00   1.00    6.00    --   95.80 -82.00  90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0484933000
_diffrn_orient_matrix_UB_12      0.0583841000
_diffrn_orient_matrix_UB_13      -0.0333979000
_diffrn_orient_matrix_UB_21      -0.0326465000
_diffrn_orient_matrix_UB_22      0.0975683000
_diffrn_orient_matrix_UB_23      -0.0255776000
_diffrn_orient_matrix_UB_31      0.0079630000
_diffrn_orient_matrix_UB_32      0.0450260000
_diffrn_orient_matrix_UB_33      0.0988401000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1504
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            40451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.066
_diffrn_reflns_theta_max         67.066
_diffrn_reflns_theta_min         3.896
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.975
_refine_diff_density_min         -4.835
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0866P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3447
_reflns_number_total             4212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08149_si_004.cif
_cod_data_source_block           exp_444
_cod_database_code               4128344
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.131
_shelx_estimated_absorpt_t_min   0.067
_reflns_odcompleteness_completeness 99.87
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B),
 C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              2590
_shelx_hkl_checksum              31973
_shelx_fab_checksum              44186
_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 5.695
_oxdiff_exptl_absorpt_empirical_full_min 0.240