π-Extended ligands with dual-binding behavior: hindered rotation unlocks unexpected reactivity in cyclometalated Pt complexes.
Ota, Seiya; Soto, Miguel A.; Patrick, Brian O.; Kamal, Saeid; Lelj, Francesco; MacLachlan, Mark J.; Chemical science 15 (2024) 14644–14650; doi:10.1039/d4sc04799k

data_1572565
_publ_section_title
;
 &#x3c0;-Extended ligands with dual-binding behavior: hindered rotation
 unlocks unexpected reactivity in cyclometalated Pt complexes.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              14644
_journal_page_last               14650
_journal_paper_doi               10.1039/d4sc04799k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C30 H20 Cl2 N2 Pt, 0.5(C H2 Cl2), 0.25[]'
_chemical_formula_sum            'C30.5 H21 Cl3 N2 Pt'
_chemical_formula_weight         716.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-21 deposited with the CCDC.	2024-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                104.299(2)
_cell_angle_beta                 95.141(2)
_cell_angle_gamma                106.641(2)
_cell_formula_units_Z            4
_cell_length_a                   11.7578(7)
_cell_length_b                   11.7959(8)
_cell_length_c                   21.4886(13)
_cell_measurement_reflns_used    6719
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.17
_cell_volume                     2725.5(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9886
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_min         1.835
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.465
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0670 before and 0.0479 after correction.
 
For component 2:
 wR2(int) was 0.0879 before and 0.0635 after correction.
 
For component 3:
 wR2(int) was 0.1115 before and 0.0870 after correction.
 The Ratio of minimum to maximum transmission is 0.77.

Final HKLF 4 output contains 113570 reflections, Rint = 0.1039
 (36409 with I > 3sig(I), Rint = 0.0580)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       plate
_exptl_crystal_F_000             1388
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max          0.95
_exptl_crystal_size_mid          0.92
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.785
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0429P)^2^+6.9554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7028
_reflns_number_total             9886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04799k2.cif
_cod_data_source_block           mo_mm567_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 1572565--1572572.cif.'
_cod_original_formula_sum        'C30.50 H21 Cl3 N2 Pt'
_cod_database_code               1572565
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.078
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34),
 C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C46(H46), C47(H47),
  C48(H48), C49(H49), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58)
;
_shelx_res_checksum              42184
_shelx_hkl_checksum              88322
_shelx_fab_checksum              9168
_platon_squeeze_void_probe_radius 1.20
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop oil'
_olex2_submission_original_sample_id NAPPtIV56
_olex2_submission_special_instructions 'No special instructions were received'