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_1550874
_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 N4 Na2 P2'
_chemical_formula_sum            'C56 H56 N4 Na2 P2'
_chemical_formula_weight         892.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-17
_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                 116.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.854(2)
_cell_length_b                   18.092(4)
_cell_length_c                   12.986(3)
_cell_measurement_reflns_used    8527
_cell_measurement_temperature    210
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      1.75
_cell_volume                     2500.4(11)
_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      210.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '2-circle diffractometer'
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.1401
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21802
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.083
_diffrn_reflns_theta_min         1.914
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.5757
_exptl_absorpt_correction_T_min  0.3606
_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    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1568 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.20(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         9684
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0088P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                5402
_reflns_number_total             9684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00629j2.cif
_cod_data_source_block           tjf053
_cod_original_cell_volume        2500.2(10)
_cod_database_code               1550874
_shelx_shelxl_version_number     2018/3
_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:
 C17(H17), C25(H25), C9(H9), C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C44(H44), C46(H46), C43(H43), C37(H37), C20(H20), C50(H50),
 C34(H34), C24(H24), C40(H40), C56(H56), C38(H38), C35(H35), C41(H41), C36(H36),
  C42(H42), C23(H23), C30(H30), C29(H29), C53(H53), C48(H48), C55(H55),
 C22(H22), C8(H8), C49(H49), C6(H6), C52(H52), C32(H32), C54(H54), C16(H16),
 C14(H14), C21(H21), C47(H47), C12(H12), C7(H7), C15(H15), C5(H5), C31(H31),
 C4(H4), C13(H13)
2.c Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C18(H18a,H18b,H18c), C26(H26a,H26b,H26c), C10(H10a,H10b,H10c)
;
_shelx_res_checksum              56370
_olex2_submission_special_instructions 'No special instructions were received'