The structure-defining incorporation of chloride in methyllithium dimers.
Knauer, Lena; Strohmann, Carsten; Chemical communications (Cambridge, England) 56 (2020) 13543–13546; doi:10.1039/d0cc05547f

data_7127384
_publ_section_title
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 The structure-defining incorporation of chloride in methyllithium dimers.
;
_journal_issue                   88
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13543
_journal_page_last               13546
_journal_paper_doi               10.1039/d0cc05547f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C27.717 H73.15 Cl0.283 Li6 N6 O'
_chemical_formula_sum            'C27.72 H73.15 Cl0.28 Li6 N6 O'
_chemical_formula_weight         558.36
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-08-04 deposited with the CCDC.	2020-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.9150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.719(2)
_cell_length_b                   9.9975(6)
_cell_length_c                   27.5561(14)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.54
_cell_volume                     7970.1(8)
_computing_cell_refinement       'SAINT V8.35A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.35A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS PHOTON100 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32957
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.169
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.8151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1321 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.9047.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.931
_exptl_crystal_description       block
_exptl_crystal_F_000             2498
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane/diethylether'
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.00099(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0671P)^2^+6.7502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5376
_reflns_number_total             7819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05547f2.cif
_cod_data_source_block           mo_b0242_0m
_cod_depositor_comments
'Adding full bibliography for 7127384--7127386.cif.'
_cod_database_code               7127384
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All Li(H,H,H) groups, All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19) = Uanis(Cl1)
3. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(H14C)=Sof(H14D)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C15A)=
 Sof(H15C)=Sof(H15D)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2)
 Sof(H14A)=Sof(H14B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C26(H26A,H26B), C12(H12A,H12B), C25(H25A,H25B), C14(H14A,
 H14B), C14(H14C,H14D), C23(H23A,H23B), C22(H22A,H22B), C3(H3A,H3B), C1(H1A,
 H1B), C15(H15A,H15B), C15A(H15C,H15D)
4.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C10(H10A,H10B,H10C), C9(H9A,H9B,
 H9C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C4(H4A,H4B,H4C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C16(H16A,
 H16B,H16C), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F)
;
_olex2_submission_special_instructions 'No special instructions were received'