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_1550876
_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         'C56 H56 Li2 N4 P2'
_chemical_formula_sum            'C56 H56 Li2 N4 P2'
_chemical_formula_weight         860.86
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-22
_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                81.58(3)
_cell_angle_beta                 88.39(3)
_cell_angle_gamma                60.36(3)
_cell_formula_units_Z            5
_cell_length_a                   12.700(3)
_cell_length_b                   12.756(3)
_cell_length_c                   43.400(9)
_cell_measurement_reflns_used    101652
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      1.42
_cell_volume                     6037(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
;
%$getVar(solution_reference_short)%
;
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            139096
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.178
_diffrn_reflns_theta_max         25.178
_diffrn_reflns_theta_min         1.425
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9664
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-Red & X-Shape & LANA'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 12483 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.00197(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2902
_refine_ls_number_reflns         41258
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0458P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.911
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                31511
_reflns_number_total             41258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00629j2.cif
_cod_data_source_block           tjf-pr08-2
_cod_database_code               1550876
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.964
_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), C73(H73), C81(H81),
 C113(H113), C121(H121), C129(H129), C137(H137), C169(H169), C177(H177),
 C185(H185), C193(H193), C225(H225), C233(H233), C241(H241), C249(H249)
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), C76(H76), C77(H77), C78(H78),
 C79(H79), C80(H80), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C90(H90),
  C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97), C98(H98),
 C99(H99), C100(H100), C102(H102), C103(H103), C104(H104), C105(H105),
 C106(H106), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112),
 C116(H116), C117(H117), C118(H118), C119(H119), C120(H120), C124(H124),
 C125(H125), C126(H126), C127(H127), C128(H128), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C140(H140), C141(H141), C142(H142),
 C143(H143), C144(H144), C146(H146), C147(H147), C148(H148), C149(H149),
 C150(H150), C152(H152), C153(H153), C154(H154), C155(H155), C156(H156),
 C158(H158), C159(H159), C160(H160), C161(H161), C162(H162), C164(H164),
 C165(H165), C166(H166), C167(H167), C168(H168), C172(H172), C173(H173),
 C174(H174), C175(H175), C176(H176), C180(H180), C181(H181), C182(H182),
 C183(H183), C184(H184), C188(H188), C189(H189), C190(H190), C191(H191),
 C192(H192), C196(H196), C197(H197), C198(H198), C199(H199), C200(H200),
 C202(H202), C203(H203), C204(H204), C205(H205), C206(H206), C208(H208),
 C209(H209), C210(H210), C211(H211), C212(H212), C214(H214), C215(H215),
 C216(H216), C217(H217), C218(H218), C220(H220), C221(H221), C222(H222),
 C223(H223), C224(H224), C228(H228), C229(H229), C230(H230), C231(H231),
 C232(H232), C236(H236), C237(H237), C238(H238), C239(H239), C240(H240),
 C244(H244), C245(H245), C246(H246), C247(H247), C248(H248), C252(H252),
 C253(H253), C254(H254), C255(H255), C256(H256), C258(H258), C259(H259),
 C260(H260), C261(H261), C262(H262), C264(H264), C265(H265), C266(H266),
 C267(H267), C268(H268), C270(H270), C271(H271), C272(H272), C273(H273),
 C274(H274), C276(H276), C277(H277), C278(H278), C279(H279), C280(H280)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C26(H26A,H26B,
 H26C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C74(H74A,H74B,H74C), C82(H82A,
 H82B,H82C), C114(H11A,H11B,H11C), C122(H12A,H12B,H12C), C130(H13A,H13B,H13C),
 C138(H13D,H13E,H13F), C170(H17A,H17B,H17C), C178(H17D,H17E,H17F), C186(H18D,
 H18E,H18F), C194(H19A,H19B,H19C), C226(H22A,H22B,H22C), C234(H23A,H23B,H23C),
 C242(H24A,H24B,H24C), C250(H25A,H25B,H25C)
;
_shelx_res_checksum              25011
_olex2_submission_special_instructions 'No special instructions were received'