Alkali metal complexes of an enantiopure iminophosphonamide ligand with bright delayed fluorescence
Feuerstein, Thomas J.; Goswami, Bhupendra; Rauthe, Pascal; Köppe, Ralf; Lebedkin, Sergei; Kappes, Manfred M.; Roesky, Peter W.; Chemical Science 10 (2019) 4742–4749; doi:10.1039/C9SC00629J

data_1550877
_publ_section_title
;
 Alkali metal complexes of an enantiopure iminophosphonamide ligand with
 bright delayed fluorescence
;
_journal_issue                   18
_journal_name_full               'Chemical Science'
_journal_page_first              4742
_journal_page_last               4749
_journal_paper_doi               10.1039/C9SC00629J
_journal_volume                  10
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '1.5(C56 H56 Cs2 N4 P2)'
_chemical_formula_sum            'C84 H84 Cs3 N6 P3'
_chemical_formula_weight         1669.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.    2019-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.693(3)
_cell_length_b                   17.008(3)
_cell_length_c                   32.906(7)
_cell_measurement_reflns_used    53826
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.72
_cell_measurement_theta_min      2.28
_cell_volume                     7663(3)
_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_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  STOE
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            42195
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.276
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.7021
_exptl_absorpt_correction_T_min  0.3437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE X-RED, X-SHAPE & LANA'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_recrystallization_method
'The material was recrystallised from hot hexane.'
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.213
_refine_diff_density_max         0.914
_refine_diff_density_min         -1.901
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 5838 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         14831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+14.6455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                13858
_reflns_number_total             14831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00629j2.cif
_cod_data_source_block           orthocs
_cod_database_code               1550877
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.627
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C9(H9), C17(H17), C25(H25), C57(H57), C65(H65)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C68(H68),
  C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76),
 C77(H77), C78(H78), C81(H81), C82(H82), C83(H83), C84(H84)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C10(H10B,H10A,H10C), C18(H18A,H18B,H18C), C26(H26A,H26B,
 H26C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              57494
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'