Experimental and theoretical studies on circularly polarized phosphorescence of a [2.2]paracyclophane-based platinum(ii) complex.
Inoue, Ryo; Kondo, Riki; Morisaki, Yasuhiro; Chemical communications (Cambridge, England) 56 (2020) 15438–15441; doi:10.1039/d0cc06205g

data_7127461
_publ_section_title
;
 Experimental and theoretical studies on circularly polarized
 phosphorescence of a [2.2]paracyclophane-based platinum(ii) complex.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15438
_journal_page_last               15441
_journal_paper_doi               10.1039/d0cc06205g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '0.53(C80 N4 O4 Pt2), 0.5(O)'
_chemical_formula_sum            'C80 H86 N4 O4 Pt2'
_chemical_formula_weight         1557.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-11 deposited with the CCDC.	2020-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.3919(17)
_cell_angle_gamma                90
_cell_formula_units_Z            15
_cell_length_a                   21.7528(3)
_cell_length_b                   51.3282(5)
_cell_length_c                   22.4375(3)
_cell_measurement_reflns_used    82265
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.7380
_cell_measurement_theta_min      2.3570
_cell_volume                     22993.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.929
_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   -120.00  60.00   0.50   54.99    --  -30.00  45.00   0.00  360
  2  \w   -120.00  60.00   0.50   54.99    --  -30.00  45.00  90.00  360
  3  \w   -120.00  60.00   0.50   54.99    --  -30.00  45.00 180.00  360
  4  \w   -120.00 -60.00   0.50   54.99    --  -30.00  45.00 270.00  120
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0189254000
_diffrn_orient_matrix_UB_12      0.0003699000
_diffrn_orient_matrix_UB_13      -0.0340387000
_diffrn_orient_matrix_UB_21      0.0035643000
_diffrn_orient_matrix_UB_22      0.0137342000
_diffrn_orient_matrix_UB_23      0.0003920000
_diffrn_orient_matrix_UB_31      0.0298494000
_diffrn_orient_matrix_UB_32      -0.0014167000
_diffrn_orient_matrix_UB_33      -0.0053498000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       67
_diffrn_reflns_limit_k_min       -66
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            218948
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_min         2.381
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       needle
_exptl_crystal_F_000             11730
_exptl_crystal_preparation       xylene/meoh
_exptl_crystal_recrystallization_method xylene/meoh
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.406(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3242
_refine_ls_number_reflns         105599
_refine_ls_number_restraints     329
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.915
_reflns_Friedel_fraction_max     0.798
_reflns_number_gt                61766
_reflns_number_total             105599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06205g2.cif
_cod_data_source_block           20200808kon
_cod_depositor_comments          'Adding full bibliography for 7127461.cif.'
_cod_original_cell_volume        22993.1(6)
_cod_database_code               7127461
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C80H86N4O4Pt2
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.655
_reflns_odcompleteness_completeness 92.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.93
_olex2_refinement_description
;
1. Restrained distances
 C63-C2L
 1.52 with sigma of 0.02
 C113-C2L
 1.52 with sigma of 0.02
 C349-C2L
 1.52 with sigma of 0.02
 C63-C349
 2.52 with sigma of 0.02
 C63-C113
 2.52 with sigma of 0.02
 C349-C113
 2.52 with sigma of 0.02
2. Rigid bond restraints
 C996, C995, C921, C923, C922, N57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2S, C997, C2U, C2Y
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2S, C997, C2Y, C2U, C923
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1J, C7, C12, C19, C3, C1Z, O23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2T, C985, C986, C2V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2M, C2D, C31, C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C274, C2Z, C2P, C868
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C972, O26, C973
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C146, C716, C492, N266, C282, C960
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C950, C951, C952, C953, C954, C873, C956, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C996 \\sim C923 \\sim C995 \\sim N57 \\sim C921 \\sim C922: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C2S \\sim C997 \\sim C2U \\sim C2Y: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C2S \\sim C997 \\sim C2Y \\sim C2U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C1J \\sim C1Z \\sim C3 \\sim C19 \\sim C7 \\sim C12 \\sim O23: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C2T \\sim C985 \\sim C986 \\sim C2V: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C2M \\sim C2D \\sim C0AA \\sim C31: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C2Z \\sim C274 \\sim C2P \\sim C868: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
O26 \\sim C973 \\sim C972: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C146 \\sim C960 \\sim C492 \\sim C282 \\sim N266 \\sim C716: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C956 \\sim C954 \\sim C953 \\sim C952 \\sim C951 \\sim C23 \\sim C873 \\sim
C950: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: O121(0.75)
;
_shelx_res_checksum              37558
_shelx_hkl_checksum              81548
_shelx_fab_checksum              46112
_olex2_exptl_crystal_mounting_method fiber
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.082
_oxdiff_exptl_absorpt_empirical_full_min 0.756