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_4122254
_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         'C81 H103 B N2 O Pt, 4.5(C6 H12)'
_chemical_formula_sum            'C108 H157 B N2 O Pt'
_chemical_formula_weight         1705.25
_chemical_name_common            Pt(kappa-2-C,N,-(PhCHO)(Cy)2BIM)(CNArDipp2)'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4844)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.4150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7728(11)
_cell_length_b                   25.8576(17)
_cell_length_c                   24.2120(15)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.399
_cell_measurement_theta_min      2.365
_cell_volume                     9422.1(11)
_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-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            76297
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         1.586
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2014/2 was used for absorption correction.
wR2(int) was 0.1380 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.6545.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         19231
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+5.7614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16621
_reflns_number_total             19231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505843g_si_002.cif
_cod_data_source_block           JFig968
_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.

'_exptl_crystal_colour_primary' value 'Violet' changed
to 'violet' 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               4122254
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.741
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C64B) = Uanis(C64)
Uanis(C23B) = Uanis(C23S)
Uanis(C24B) = Uanis(C24S)
Uanis(C19S) = Uanis(C19B)
Uanis(C20S) = Uanis(C20B)
Uanis(C21S) = Uanis(C21B)
Uanis(C22S) = Uanis(C22B)
3. Rigid body (RIGU) restrains
 C64, C64B, C66, C66B, C65, C65B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28S, C25S, C26S, C30S, C27S, C29S
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
4. Same fragment restrains
{C1S, C2S, C3S, C4S, C5S, C6S}
as
{C19S, C20S, C21S, C22S, C23S, C24S}
{C1S, C2S, C3S, C4S, C5S, C6S}
as
{C19B, C20B, C21B, C22B, C23B, C24B}
{C1S, C2S, C3S, C4S, C5S, C6S}
as
{C25S, C26S, C27S, C28S, C29S, C30S}
5. Others
 Sof(C65B)=Sof(H65D)=Sof(H65E)=Sof(H65F)=Sof(C66B)=Sof(H66D)=Sof(H66E)=
 Sof(H66F)=1-FVAR(1)
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=
 FVAR(1)
 Sof(C64)=Sof(H64)=1-FVAR(2)
 Sof(C64B)=Sof(H64B)=FVAR(2)
 Fixed Sof: C19S(0.5) H19A(0.5) H19B(0.5) C20S(0.5) H20D(0.5) H20E(0.5)
 C21S(0.5) H21D(0.5) H21E(0.5) C22S(0.5) H22A(0.5) H22B(0.5) C23S(0.5)
 H23A(0.5) H23B(0.5) C24S(0.5) H24A(0.5) H24B(0.5) C19B(0.5) H19C(0.5)
 H19D(0.5) C20B(0.5) H20F(0.5) H20G(0.5) C21B(0.5) H21F(0.5) H21G(0.5)
 C22B(0.5) H22C(0.5) H22D(0.5) C23B(0.5) H23C(0.5) H23D(0.5) C24B(0.5)
 H24C(0.5) H24D(0.5) C25S(0.5) H25A(0.5) H25B(0.5) C26S(0.5) H26A(0.5)
 H26B(0.5) C27S(0.5) H27A(0.5) H27B(0.5) C28S(0.5) H28A(0.5) H28B(0.5)
 C29S(0.5) H29D(0.5) H29E(0.5) C30S(0.5) H30D(0.5) H30E(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C3(H3), C16(H16), C19(H19), C28(H28), C31(H31), C34(H34), C46(H46),
 C67(H67), C76(H76), C79(H79), C64(H64), C64B(H64B)
6.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
 C51(H51A,H51B), C19S(H19A,H19B), C20S(H20D,H20E), C21S(H21D,H21E), C22S(H22A,
 H22B), C23S(H23A,H23B), C24S(H24A,H24B), C19B(H19C,H19D), C20B(H20F,H20G),
 C21B(H21F,H21G), C22B(H22C,H22D), C23B(H23C,H23D), C24B(H24C,H24D), C1S(H1SA,
 H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB),
 C6S(H6SA,H6SB), C7S(H7SA,H7SB), C8S(H8SA,H8SB), C9S(H9SA,H9SB), C10S(H10A,
 H10B), C11S(H11A,H11B), C12S(H12A,H12B), C13S(H13A,H13B), C14S(H14A,H14B),
 C15S(H15A,H15B), C16S(H16A,H16B), C17S(H17D,H17E), C18S(H18D,H18E), C25S(H25A,
 H25B), C26S(H26A,H26B), C27S(H27A,H27B), C28S(H28A,H28B), C29S(H29D,H29E),
 C30S(H30D,H30E)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C54(H54), C55(H55),
  C56(H56), C60(H60), C61(H61), C62(H62), C72(H72), C73(H73), C74(H74)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C77(H77A,H77B,H77C),
 C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C65B(H65D,H65E,H65F), C66B(H66D,H66E,H66F)
;
_shelx_res_checksum              47585
_shelx_hkl_checksum              92445
_olex2_submission_special_instructions 'No special instructions were received'