Activation of heteroallenes by coordinatively unsaturated nickel(ii) alkyl complexes supported by the hydrotris(3-phenyl-5-methyl)pyrazolyl borate (Tp(Ph,Me)) ligand.
Abubekerov, Mark; Eymann, Léonard Y M; Gianetti, Thomas L.; Arnold, John; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14581–14590; doi:10.1039/c6dt01585a

data_7039649
_publ_section_title
;
 Activation of heteroallenes by coordinatively unsaturated nickel(ii)
 alkyl complexes supported by the hydrotris(3-phenyl-5-methyl)pyrazolyl
 borate (Tp(Ph,Me)) ligand.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14581
_journal_page_last               14590
_journal_paper_doi               10.1039/c6dt01585a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C35 H39 B N6 Ni S2 Si, C5.97 H17.91 O0.995 Si1.99'
_chemical_formula_sum            'C40.97 H56.91 B N6 Ni O S2 Si2.99'
_chemical_formula_weight         867.02
_chemical_melting_point          448.7(5)
_chemical_name_systematic        'Complex 2b'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2016-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-07 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                112.175(4)
_cell_angle_beta                 101.588(4)
_cell_angle_gamma                98.702(4)
_cell_formula_units_Z            2
_cell_length_a                   10.534(9)
_cell_length_b                   15.566(7)
_cell_length_c                   17.689(9)
_cell_measurement_reflns_used    8049
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.33
_cell_volume                     2547(3)
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30732
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.387
_diffrn_reflns_theta_min         1.488
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_T_min  0.8261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0428 after correction.
The Ratio of minimum to maximum transmission is 0.9175.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rode
_exptl_crystal_F_000             919
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9357
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1053P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.1978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5732
_reflns_number_total             9357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01585a1.cif
_cod_data_source_block           Complex_2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '448.2 - 449.2' was changed to
'448.7(5)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039640--7039649.cif.
;
_cod_original_cell_volume        2547.9(23)
_cod_database_code               7039649
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1A-C41 \\sim Si1A-C42 \\sim Si1A-O0AA \\sim Si1A-C40 \\sim Si3-C38 \\sim
Si3-C37 \\sim Si3-C36
 with sigma of 0.02
 Si1A-O0AA \\sim Si3-O0AA
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C42, C41, Si1A, C40, O0AA, Si3, C38, C37, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C41, Si1A, O0AA, Si3, C38, C37, C36, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(Si1A)=Sof(O0AA)=Sof(Si3)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 B1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB)
5.c Me refined with riding coordinates:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
5.d Aromatic/amide H refined with riding coordinates:
 C6AA(H6AA), C8AA(H8AA), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35)
5.e Idealised Me refined as rotating group:
 C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C4AA(H4AA,H4AB,H4AC), C5AA(H5AA,
 H5AB,H5AC), C16(H16A,H16B,H16C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method 'Hexamethyl disiloxane'