Frustrated Lewis pairs with thermally activated delayed fluorescence properties: activation of formaldehyde.
Lee, Young Hoon; Nam, Eun Bi; Lee, Junseong; Lee, Sang Uck; Lee, Min Hyung; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13198–13201; doi:10.1039/d0dt02507k

data_7704977
_publ_section_title
;
 Frustrated Lewis pairs with thermally activated delayed fluorescence
 properties: activation of formaldehyde.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13198
_journal_page_last               13201
_journal_paper_doi               10.1039/d0dt02507k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C67 H45 B2 F15 N O P, 2(C2 H5 O0.5)'
_chemical_formula_sum            'C71 H55 B2 F15 N O2 P'
_chemical_formula_weight         1291.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014-3
_audit_update_record
;
2020-07-30 deposited with the CCDC.	2020-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6709(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2411(3)
_cell_length_b                   23.1001(5)
_cell_length_c                   20.8633(4)
_cell_measurement_reflns_used    9274
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.639
_cell_measurement_theta_min      2.287
_cell_volume                     6744.7(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            105922
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.783
_diffrn_reflns_theta_min         2.383
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0915 before and 0.0463 after correction. The Ratio of minimum to maximum transmission is 0.8360. The \l/2 correction factor is 0.00150.'
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         12902
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1452P)^2^+5.2672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9872
_reflns_number_total             12902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02507k2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7704977.cif.'
_cod_database_code               7704977
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C69A-O2
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C52) \\sim Ueq, Uanis(C52A) \\sim Ueq, Uanis(C54A) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C75A) \\sim Ueq,
Uanis(C51A) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C55A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: F1(0.5) F1A(0.5) O2(0.5) O3(0.5) C68(0.5) H68A(0.3) H68B(0.3)
 H68C(0.3) H68D(0.2) H68E(0.2) H68F(0.2) C71(0.5) H71A(0.3) H71B(0.3) H71C(0.3)
 H71D(0.2) H71E(0.2) H71F(0.2) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) C74(0.5) H74A(0.25) H74B(0.25) H74C(0.25) H74D(0.25)
 F4(0.5) F3(0.5) F2(0.5) F5(0.5) N1(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5)
 C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5)
 H7(0.5) C8(0.5) H8(0.5) C9(0.5) C10(0.5) C11(0.5) C12(0.5) C51(0.5) C52(0.5)
 C53(0.5) C54(0.5) C55(0.5) C50(0.5) C69(0.3) H69A(0.3) H69B(0.3) C70(0.3)
 H70A(0.3) H70B(0.3) C75(0.25) H75A(0.25) H75B(0.25) H75C(0.25) F2A(0.5)
 F3A(0.5) F4A(0.5) F5A(0.5) N1A(0.5) C1A(0.5) H1A(0.5) C69A(0.2) H69C(0.2)
 H69D(0.2) C2A(0.5) H2A(0.5) C75A(0.25) H75D(0.25) H75E(0.25) H75F(0.25)
 C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5)
 C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) C10A(0.5) C11A(0.5) C12A(0.5)
 C50A(0.5) C55A(0.5) C54A(0.5) C53A(0.5) C52A(0.5) C51A(0.5) C70A(0.2)
 H70C(0.2) H70D(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C73(H73A,H73B), C74(H74A,H74B), C74(H74C,H74D), C69(H69A,
 H69B), C70(H70A,H70B), C69A(H69C,H69D), C70A(H70C,H70D)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C17(H17), C21(H21), C23(H23), C30(H30), C32(H32),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7),
 C8(H8), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A),
 C8A(H8A)
5.c Fitted hexagon refined as free rotating group:
 C51(C52,C53,C54,C55,C50), C50A(C55A,C54A,C53A,C52A,C51A)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C68(H68A,H68B,H68C), C68(H68D,
 H68E,H68F), C71(H71A,H71B,H71C), C71(H71D,H71E,H71F), C72(H72A,H72B,H72C),
 C75(H75A,H75B,H75C), C75A(H75D,H75E,H75F)
;
_shelx_res_checksum              95767
_olex2_submission_special_instructions 'No special instructions were received'