Bright Luminescent Lithium and Magnesium Carbene Complexes
Pinter, Piermaria; Schuesslbauer, Christoph; Watt, Fabian A.; Dickmann, Nicole; Herbst-Irmer, Regine; Morgenstern, Bernd; Gruenwald, Annette; Ullrich, Tobias; Zimmer, Michael; Hohloch, Stephan; Guldi, Dirk M.; Munz, Dominik; Chemical Science  (2021) –; doi:10.1039/D1SC00846C

data_1561844
_publ_section_title
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 Bright Luminescent Lithium and Magnesium Carbene Complexes
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC00846C
_journal_year                    2021
_chemical_formula_moiety         'I, C32 H40 N7, 6(C3 H3)'
_chemical_formula_sum            'C50 H58 I N7'
_chemical_formula_weight         883.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-01 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
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_cell_angle_alpha                113.980(2)
_cell_angle_beta                 96.942(2)
_cell_angle_gamma                105.305(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5612(6)
_cell_length_b                   15.8193(9)
_cell_length_c                   15.8498(8)
_cell_measurement_reflns_used    5776
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.20
_cell_volume                     2254.1(2)
_computing_cell_refinement       'Bruker Apex3 suite, 2020'
_computing_data_collection       'Bruker Apex3 suite, 2020'
_computing_data_reduction        'Bruker Apex3 suite, 2020'
_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      153.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'omega phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1527
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54094
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.467
_diffrn_reflns_theta_min         2.201
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0991 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.9066.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8291
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0348P)^2^+1.6272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5776
_reflns_number_total             8291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00846c2.cif
_cod_data_source_block           sh_sh_15_0m
_cod_database_code               1561844
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   'Blessing, 1995'
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C200-C201
 1.49 with sigma of 0.01
 C201-C202
 1.49 with sigma of 0.01
 C100-C101
 1.49 with sigma of 0.01
 C101-C102
 1.49 with sigma of 0.01
 C102-C103
 1.49 with sigma of 0.01
 C103-C104
 1.49 with sigma of 0.01
 C104-C105
 1.49 with sigma of 0.01
 C105-C100
 1.49 with sigma of 0.01
 C300-C301
 1.49 with sigma of 0.01
 C301-C302
 1.49 with sigma of 0.01
 C302-C303
 1.49 with sigma of 0.01
 C303-C304
 1.49 with sigma of 0.01
 C304-C305
 1.49 with sigma of 0.01
 C305-C300
 1.49 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B),
 C11(H11A,H11B), C6(H6A,H6B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C1(H1), C2(H2), C21(H21), C23(H23), C401(H401),
 C402(H402), C400(H400), C105(H105), C104(H104), C100(H100), C101(H101),
 C103(H103), C102(H102), C201(H201), C200(H200), C202(H202), C302(H302),
 C301(H301), C303(H303), C304(H304), C300(H300), C305(H305)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
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_olex2_submission_special_instructions 'No special instructions were received'