Cooperative Transition Metal/Lewis Acid Bond-Activation Reactions by a Bidentate (Boryl)iminomethane Complex: A Significant Metal-Borane Interaction Promoted by a Small Bite-Angle LZ Chelate.
Barnett, Brandon R.; Moore, Curtis E.; Rheingold, Arnold L.; Figueroa, Joshua S.; Journal of the American Chemical Society 136 (2014) 10262–10265; doi:10.1021/ja505843g

data_4122251
_publ_section_title
;
 Cooperative Transition Metal/Lewis Acid Bond-Activation Reactions by a
 Bidentate (Boryl)iminomethane Complex: A Significant Metal-Borane
 Interaction Promoted by a Small Bite-Angle LZ Chelate.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10262
_journal_page_last               10265
_journal_paper_doi               10.1021/ja505843g
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C43 H60 B2 Cl3 N, 2(C5 H12)'
_chemical_formula_sum            'C53 H84 B2 Cl3 N'
_chemical_formula_weight         863.18
_chemical_name_common            '[Cy2BIM][BCl3]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.980(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1651(12)
_cell_length_b                   18.0874(13)
_cell_length_c                   18.8461(12)
_cell_measurement_reflns_used    6687
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.209
_cell_measurement_theta_min      2.505
_cell_volume                     5091.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37218
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.434
_diffrn_reflns_theta_min         1.363
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0810 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.8811.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         9393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0887P)^2^+1.4472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6432
_reflns_number_total             9393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505843g_si_002.cif
_cod_data_source_block           JFig937
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/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 

 Adding full bibliography for 4122242--4122254.cif.
;
_cod_database_code               4122251
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.942
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C20)
Uanis(C38B) = Uanis(C38)
Uanis(C40B) = Uanis(C40)
Uanis(C41B) = Uanis(C41)
Uanis(C42B) = Uanis(C42)
Uanis(C43B) = Uanis(C43)
Uanis(C9SB) = Uanis(C9S)
Uanis(C8SB) = Uanis(C8S)
3. Others
 Sof(H7SC)=Sof(H7SD)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C8SB)=Sof(H8SC)=
 Sof(H8SD)=Sof(C9SB)=Sof(H9SC)=Sof(H9SD)=1-FVAR(1)
 Sof(H7SA)=Sof(H7SB)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C8S)=Sof(H8SA)=
 Sof(H8SB)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=FVAR(1)
 Sof(H39C)=Sof(H39D)=Sof(C38B)=Sof(H38B)=Sof(C40B)=Sof(H40C)=Sof(H40D)=
 Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=
 Sof(H43C)=Sof(H43D)=1-FVAR(2)
 Sof(H39A)=Sof(H39B)=Sof(C38)=Sof(H38)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C26(H26), C29(H29), C32(H32), C38(H38), C38B(H38B)
4.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C39(H39A,H39B), C39(H39C,H39D), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C40B(H40C,H40D), C41B(H41C,H41D), C42B(H42C,
 H42D), C43B(H43C,H43D), C7S(H7SA,H7SB), C7S(H7SC,H7SD), C8S(H8SA,H8SB),
 C9S(H9SA,H9SB), C8SB(H8SC,H8SD), C9SB(H9SC,H9SD), C2S(H2SA,H2SB), C3S(H3SA,
 H3SB), C4S(H4SA,H4SB)
4.c Me refined with riding coordinates:
 C10B(H10A,H10B,H10C), C10B(H10D,H10E,H10F)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C22(H22),
 C23(H23), C24(H24)
4.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C6S(H6SA,H6SB,H6SC), C1S(H1SA,H1SB,H1SC), C5S(H5SA,H5SB,H5SC)
;
_shelx_res_checksum              79674
_shelx_hkl_checksum              12623