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_1550875
_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 K2 N4 P2'
_chemical_formula_sum            'C56 H56 K2 N4 P2'
_chemical_formula_weight         925.18
_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   geom
_audit_creation_date             2018-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_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                   12.481(3)
_cell_length_b                   13.110(3)
_cell_length_c                   30.547(6)
_cell_measurement_reflns_used    49647
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      1.69
_cell_volume                     4998.3(19)
_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
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            41667
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.051
_diffrn_reflns_theta_min         1.690
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_correction_T_min  0.3664
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-SHAPE & X-RED & LANA'
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 3947 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         9830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0530P)^2^+0.2966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                9252
_reflns_number_total             9830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00629j2.cif
_cod_data_source_block           bg018
_cod_original_cell_volume        4998.3(17)
_cod_database_code               1550875
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.916
_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:
 C25(H25), C17(H17), C9(H9), C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C56(H56), C50(H50), C52(H52), C49(H49), C38(H38), C28(H28), C29(H29),
 C34(H34), C44(H44), C24(H24), C46(H46), C55(H55), C54(H54), C35(H35), C47(H47),
  C53(H53), C40(H40), C16(H16), C30(H30), C12(H12), C37(H37), C5(H5), C32(H32),
 C14(H14), C13(H13), C48(H48), C36(H36), C4(H4), C21(H21), C41(H41), C8(H8),
 C22(H22), C15(H15), C42(H42), C23(H23), C20(H20), C31(H31), C6(H6), C43(H43),
 C7(H7)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C26(H26A,H26B,H26C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              95781
_olex2_submission_special_instructions 'No special instructions were received'