Rotational isomerization: Spontaneous structural transformation of a thermally activated delayed fluorescence binuclear copper(I) complex
Zhang, Xiaowen; Huang, Chun-Hua; Yang, Mingxue; Chen, Xu-Lin; Lu, Can-Zhong; Dalton Transactions  (2023) –; doi:10.1039/D3DT01258A

data_7713355
_publ_section_title
;
 Rotational isomerization: Spontaneous structural transformation of a
 thermally activated delayed fluorescence binuclear copper(I) complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01258A
_journal_year                    2023
_chemical_formula_moiety         'C58 H42 Cu2 I2 N4 P2'
_chemical_formula_sum            'C58 H42 Cu2 I2 N4 P2'
_chemical_formula_weight         1237.77
_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
_audit_creation_date             2021-12-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-29 deposited with the CCDC.	2023-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                97.34(14)
_cell_angle_beta                 101.29(13)
_cell_angle_gamma                112.57(11)
_cell_formula_units_Z            2
_cell_length_a                   10.67(5)
_cell_length_b                   13.79(6)
_cell_length_c                   23.49(10)
_cell_measurement_reflns_used    4444
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.206
_cell_measurement_theta_min      2.368
_cell_volume                     3050(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_number            13476
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.045
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0925 before and 0.0656 after correction.
 
For component 2:
 wR2(int) was 0.0816 before and 0.0591 after correction.
 The Ratio of minimum to maximum transmission is 0.90.

Final HKLF 4 output contains 116728 reflections, Rint = 0.1048
 (39151 with I > 3sig(I), Rint = 0.0489)
;
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.235
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         13476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0806
_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^)+(0.0468P)^2^+16.4819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8103
_reflns_number_total             13476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01258a2.cif
_cod_data_source_block           mo_cu_g_1_0m_4_a
_cod_original_cell_volume        3051(24)
_cod_database_code               7713355
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.762
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.042) H56(0.059) H57(0.074) H4(0.051) H8(0.058) H9(0.071)
 H10(0.079) H11(0.082) H12(0.058) H14(0.045) H15(0.047) H16(0.054) H17(0.064)
 H18(0.048) H19(0.044) H20(0.047) H21(0.05) H23(0.06) H24(0.071) H25(0.067)
 H26(0.057) H31(0.046) H32(0.045) H33(0.039) H35(0.046) H36(0.053) H37(0.056)
 H38(0.065) H39(0.05) H41(0.056) H42(0.08) H43(0.084) H44(0.077) H45(0.066)
 H48(0.046) H49(0.063) H50(0.066) H51(0.054) H52(0.066) H53(0.067) H54(0.066)
 H55(0.048)
 Fixed X: H1(0.812338) H56(0.839174) H57(0.762535) H4(0.647821) H8(1.160927)
 H9(1.313429) H10(1.264383) H11(1.056419) H12(0.902443) H14(0.896855)
 H15(1.023238) H16(1.183922) H17(1.212419) H18(1.088921) H19(0.839136)
 H20(0.650547) H21(0.443421) H23(0.215929) H24(0.075488) H25(0.160496)
 H26(0.389862) H31(0.930994) H32(0.871675) H33(0.726921) H35(0.424732)
 H36(0.188373) H37(0.020564) H38(0.089875) H39(0.324261) H41(0.430935)
 H42(0.473103) H43(0.681747) H44(0.842521) H45(0.797086) H48(0.663521)
 H49(0.797089) H50(0.949947) H51(0.969744) H52(0.432423) H53(0.234351)
 H54(0.235161) H55(0.426957)
 Fixed Y: H1(0.264594) H56(0.111008) H57(0.025316) H4(0.0933) H8(0.575219)
 H9(0.7503) H10(0.892659) H11(0.858519) H12(0.683498) H14(0.332938)
 H15(0.232232) H16(0.22589) H17(0.315072) H18(0.418579) H19(0.561329)
 H20(0.527144) H21(0.3776) H23(0.185517) H24(0.029699) H25(-0.0318)
 H26(0.064759) H31(0.390156) H32(0.533205) H33(0.565415) H35(0.327652)
 H36(0.22174) H37(0.220908) H38(0.323708) H39(0.426873) H41(0.574345)
 H42(0.753156) H43(0.891459) H44(0.854812) H45(0.678202) H48(0.073392) H49(-
 0.016034) H50(0.054375) H51(0.208974) H52(0.094724) H53(0.019566)
 H54(0.102483) H55(0.256709)
 Fixed Z: H1(0.750622) H56(0.721817) H57(0.622862) H4(0.553215) H8(0.593756)
 H9(0.598696) H10(0.635302) H11(0.660775) H12(0.655674) H14(0.519776)
 H15(0.505847) H16(0.5843) H17(0.681193) H18(0.695786) H19(0.520426)
 H20(0.439673) H21(0.423985) H23(0.427688) H24(0.451837) H25(0.530245)
 H26(0.591272) H31(1.051557) H32(1.069119) H33(0.994678) H35(0.936273)
 H36(0.923985) H37(0.844492) H38(0.777836) H39(0.787353) H41(0.926882)
 H42(0.964858) H43(0.964279) H44(0.921273) H45(0.882172) H48(0.808226)
 H49(0.847364) H50(0.942528) H51(1.000801) H52(0.852793) H53(0.771978)
 H54(0.691095) H55(0.694855)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 190 electrons were 
found in a volume of 799\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[CH2Cl2], 1.5[CH3CN] per Asymmetric Unit 
which account for 192 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              659
_shelx_hkl_checksum              72136
_shelx_fab_checksum              42278
_olex2_submission_special_instructions 'No special instructions were received'