The smaller, the better? How the aggregate size affects the reactivity of (trimethylsilyl)methyllithium.
Knauer, Lena; Wattenberg, Jonathan; Kroesen, Ulrike; Strohmann, Carsten; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11285–11291; doi:10.1039/c9dt02182e

data_7700250
_publ_section_title
;
 The smaller, the better? How the aggregate size affects the reactivity of
 (trimethylsilyl)methyllithium.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11285
_journal_page_last               11291
_journal_paper_doi               10.1039/c9dt02182e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C29 H61 Li2 N3 Si2), C7 H13 N'
_chemical_formula_sum            'C65 H135 Li4 N7 Si4'
_chemical_formula_weight         1154.91
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Pyrophoric
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-21 deposited with the CCDC.    2019-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.610(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.750(3)
_cell_length_b                   12.1145(15)
_cell_length_c                   31.140(5)
_cell_measurement_reflns_used    9351
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.52
_cell_volume                     7902.5(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_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 0.995
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE area detector'
_diffrn_measurement_method       '\w and \f 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  0.0602
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            50164
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.576
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.5644
_exptl_absorpt_correction_T_min  0.4562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1626 before and 0.0939 after correction. The Ratio of minimum to maximum transmission is 0.6167. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.971
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.771
_exptl_crystal_size_mid          0.459
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         11922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0918P)^2^+17.9710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.1988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8914
_reflns_number_total             11922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02182e2.cif
_cod_data_source_block           b0373
_cod_depositor_comments
'Adding full bibliography for 7700249--7700251.cif.'
_cod_original_cell_volume        7902.4(19)
_cod_database_code               7700250
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C30) = Uanis(N4)
3. Others
 Fixed Sof: N4(0.5) C30(0.5) H30(0.5) H31A(0.5) H31B(0.5) H31C(0.5) H31D(0.5)
 H32A(0.5) H32B(0.5) H32C(0.5) H32D(0.5) H33A(0.5) H33B(0.5) H33C(0.5) H33D(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C18(H18), C25(H25), C30(H30)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C31(H31C,H31D),
 C32(H32A,H32B), C32(H32C,H32D), C33(H33A,H33B), C33(H33C,H33D)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'