Isolation and characterization of a lithiated pyridine - aggregation in the solid state and in solution.
Schmidlin, Nadja M. C.; Scherer, Harald; Hoffmann, Anke; Böttcher, Tobias; Chemical communications (Cambridge, England) 56 (2020) 4160–4163; doi:10.1039/d0cc01355b

data_7126233
_publ_section_title
;
 Isolation and characterization of a lithiated pyridine - aggregation in
 the solid state and in solution.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4160
_journal_page_last               4163
_journal_paper_doi               10.1039/d0cc01355b
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C66 H88 Li2 N2 O5'
_chemical_formula_weight         1003.26
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif by Daniel Kratzert, Freiburg 2019,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2020-02-04 deposited with the CCDC.	2020-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.779(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.845(2)
_cell_length_b                   16.759(3)
_cell_length_c                   14.762(3)
_cell_measurement_reflns_used    9431
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.7835
_cell_measurement_theta_min      2.4395
_cell_volume                     3026.0(10)
_computing_cell_refinement       'SAINT V8.38A'
_computing_data_collection       'Bruker BIS V6.2.11/2019-03-14'
_computing_data_reduction        'SAINT V8.38A'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 HPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
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_diffrn_reflns_point_group_measured_fraction_full 0.518
_diffrn_reflns_point_group_measured_fraction_max 0.513
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.889
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.745618
_exptl_absorpt_correction_T_min  0.700525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1: Krause, L.,
Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.252
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   -3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         7419
_refine_ls_number_restraints     1212
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0773
_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^)+(0.0883P)^2^+5.3509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2194
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                7116
_reflns_number_total             7419
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
'The data was integrated as a 2-component twin.'
_twin_individual_id              2
_twin_individual_twin_matrix_11  0.20004
_twin_individual_twin_matrix_12  -0.00037
_twin_individual_twin_matrix_13  -0.80077
_twin_individual_twin_matrix_21  -1e-05
_twin_individual_twin_matrix_22  -1.0
_twin_individual_twin_matrix_23  0.00055
_twin_individual_twin_matrix_31  -1.19883
_twin_individual_twin_matrix_32  6e-05
_twin_individual_twin_matrix_33  -0.20004
_cod_data_source_file            d0cc01355b2.cif
_cod_data_source_block           TB_TB292_v1_0m_4_a
_cod_depositor_comments          'Adding full bibliography for 7126233.cif.'
_cod_original_cell_volume        3025.8(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7126233
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.983
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              76871
_shelx_hkl_checksum              28232