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_4122245
_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         'C74 H97 B N2 Pt, 0.5(C5 H12)'
_chemical_formula_sum            'C76.5 H103 B N2 Pt'
_chemical_formula_weight         1256.50
_chemical_name_common            Pt(kappa-2-N,B-(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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-03
_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                 99.809(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.221(2)
_cell_length_b                   21.092(3)
_cell_length_c                   22.585(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.259
_cell_measurement_theta_min      2.342
_cell_volume                     6675.3(16)
_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      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94869
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.470
_diffrn_reflns_theta_min         1.830
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1188 before and 0.0456 after correction.
The Ratio of minimum to maximum transmission is 0.6491.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_colour_modifier   Pale
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         13649
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+7.4384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10916
_reflns_number_total             13649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505843g_si_002.cif
_cod_data_source_block           JFig877
_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 'Yellow' changed
to 'yellow' 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_original_cell_volume        6675.5(16)
_cod_original_formula_sum        'C76.50 H103 B N2 Pt'
_cod_database_code               4122245
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.594
_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. Restrained distances
 C1S-C2S = C4S-C3S = C4S-C5S
 1.54 with sigma of 0.02
 C3S-C2S
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C63) = Uanis(C63B)
Uanis(B1) = Uanis(B1B)
Uanis(C69) = Uanis(C69B)
4. Rigid body (RIGU) restrains
 Pt1, C1, C74, C63, C64, C69, C70, C72, C73, C67, B1, C71, C68, C66, C65, C74B,
  C69B, C70B, C71B, C73, C73B, C65B, C64B, C63B, C68B, C67B, C66B, B1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1S, C2S, C3S, C4S, C5S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C63B)=Sof(H63B)=Sof(C64B)=Sof(H64C)=Sof(H64D)=Sof(C65B)=Sof(H65C)=
 Sof(H65D)=Sof(C66B)=Sof(H66C)=Sof(H66D)=Sof(C67B)=Sof(H67C)=Sof(H67D)=
 Sof(C68B)=Sof(H68C)=Sof(H68D)=Sof(C69B)=Sof(H69B)=Sof(C70B)=Sof(H70C)=
 Sof(H70D)=Sof(C71B)=Sof(H71C)=Sof(H71D)=Sof(C72B)=Sof(H72C)=Sof(H72D)=
 Sof(C73B)=Sof(H73C)=Sof(H73D)=Sof(C74B)=Sof(H74C)=Sof(H74D)=Sof(B1B)=1-FVAR(1)
 Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C65)=Sof(H65A)=Sof(H65B)=
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=
 Sof(H68B)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=
 Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=
 Sof(H74A)=Sof(H74B)=Sof(B1)=FVAR(1)
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) H5SC(0.5)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C27(H27), C30(H30), C45(H45), C48(H48), C57(H57),
 C60(H60), C63(H63), C69(H69), C63B(H63B), C69B(H69B)
6.b Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,
 H68B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B),
 C74(H74A,H74B), C64B(H64C,H64D), C65B(H65C,H65D), C66B(H66C,H66D), C67B(H67C,
 H67D), C68B(H68C,H68D), C70B(H70C,H70D), C71B(H71C,H71D), C72B(H72C,H72D),
 C73B(H73C,H73D), C74B(H74C,H74D), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,
 H4SB)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C23(H23), C24(H24),
 C25(H25), C35(H35), C36(H36), C37(H37), C41(H41), C42(H42), C43(H43), C53(H53),
  C54(H54), C55(H55)
6.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C1S(H1SA,H1SB,H1SC), C5S(H5SA,H5SB,H5SC)
;
_shelx_res_checksum              3475
_shelx_hkl_checksum              12539