Ligand-assisted nickel-catalysed sp3–sp3 homocoupling of unactivated alkyl bromides and its application to the active template synthesis of rotaxanes
Goldup, Stephen M.; Leigh, David A.; McBurney, Roy T.; McGonigal, Paul R.; Plant, Andrew; Chemical Science 1 (2010) 383–; doi:10.1039/c0sc00279h

data_1515809
_publ_section_title
;
 Ligand-assisted nickel-catalysed sp3--sp3 homocoupling of unactivated
 alkyl bromides and its application to the active template synthesis of
 rotaxanes
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              383
_journal_paper_doi               10.1039/c0sc00279h
_journal_volume                  1
_journal_year                    2010
_chemical_formula_moiety         'C35 H51 N3 O6 Si2.(H2 O)0.5'
_chemical_formula_sum            'C35 H52 N3 O6.5 Si2'
_chemical_formula_weight         674.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.478(3)
_cell_angle_beta                 88.638(3)
_cell_angle_gamma                78.940(3)
_cell_formula_units_Z            4
_cell_length_a                   10.1290(6)
_cell_length_b                   18.6652(11)
_cell_length_c                   21.5360(13)
_cell_measurement_reflns_used    27529
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      1.06
_cell_volume                     3867.0(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35807
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4884
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0039(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         13692
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+3.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                12018
_reflns_number_total             13692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00279h.txt
_cod_data_source_block           dled112
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-09-24

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C35 H52 N3 O6.50 Si2'
_cod_database_code               1515809