Platinum-mediated B‒H methoxylation of bis(pyrazolyl)borate
Pal, Shrinwantu; Patrick, Brian O.; Love, Jennifer A.; Faraday Discussions  (2019) –; doi:10.1039/C9FD00052F

data_1552354
_publ_section_title
;
 Platinum-mediated B--H methoxylation of bis(pyrazolyl)borate
;
_journal_name_full               'Faraday Discussions'
_journal_paper_doi               10.1039/C9FD00052F
_journal_year                    2019
_chemical_formula_moiety         '0.5(C52 H68 B2 K2 N8 O4 Pt2)'
_chemical_formula_sum            'C26 H34 B K N4 O2 Pt'
_chemical_formula_weight         679.57
_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     dual
_audit_creation_date             2018-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-25 deposited with the CCDC.    2019-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.8910(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.6073(5)
_cell_length_b                   15.6781(9)
_cell_length_c                   35.365(2)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.52
_cell_volume                     5307.4(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_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 0.999
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            59453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.563
_diffrn_reflns_theta_min         1.422
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.475
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction. wR2(int) was 0.0840 before and 0.0460 after correction. The ratio of minimum to maximum transmission is 0.7853. The \l/2 correction factor is not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       blade
_exptl_crystal_F_000             2688
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of THF and hexanes  by slow evaporation'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.274
_refine_diff_density_min         -1.957
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         16275
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+9.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12183
_reflns_number_total             16275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00052f2.cif
_cod_data_source_block           jl312
_cod_original_cell_volume        5307.5(5)
_cod_database_code               1552354
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.366
_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
2. Restrained distances
 O1-C23 \\sim O2-C22A \\sim O2-C22 \\sim O2-C19
 with sigma of 0.01
 C24-C23 \\sim C22A-C21 \\sim C22-C21A \\sim C20A-C19 \\sim C20-C19
 with sigma of 0.01
 C25-C24 \\sim C21-C20 \\sim C20A-C21A
 with sigma of 0.01
 O3-C52 \\sim O4-C48 \\sim O4-C48A \\sim O4-C45
 with sigma of 0.01
 C52-C51 \\sim C48A-C47A \\sim C48-C47 \\sim C46-C45 \\sim C46A-C45
 with sigma of 0.01
 C51-C50 \\sim C47-C46 \\sim C47A-C46A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O2 \\sim C19 \\sim C20 \\sim C20A \\sim C21 \\sim C21A \\sim C22A \\sim C22
\\sim C22A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O4 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C46A \\sim C47A \\sim C48A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C20A) = Uanis(C20)
4. Rigid body (RIGU) restrains
 O2, C19, C20, C20A, C21, C21A, C22A, C22, C22A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C45, C46, C47, C48, C46A, C47A, C48A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H19C)=Sof(H19D)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(C22)=Sof(H22C)=Sof(H22D)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21C)=
 Sof(H21D)=Sof(C22A)=Sof(H22A)=Sof(H22B)=FVAR(1)
 Sof(H45C)=Sof(H45D)=Sof(C46)=Sof(H46C)=Sof(H46D)=Sof(C47)=Sof(H47C)=Sof(H47D)=
 Sof(C48)=Sof(H48C)=Sof(H48D)=1-FVAR(2)
 Sof(H45A)=Sof(H45B)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(C47A)=Sof(H47A)=
 Sof(H47B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C19(H19C,H19D), C19(H19A,H19B), C20(H20A,H20B), C20A(H20C,H20D), C21(H21A,
 H21B), C21A(H21C,H21D), C22A(H22A,H22B), C22(H22C,H22D), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C45(H45A,H45B), C45(H45C,H45D),
  C46A(H46A,H46B), C47A(H47A,H47B), C48A(H48A,H48B), C49(H49A,H49B), C50(H50A,
 H50B), C51(H51A,H51B), C52(H52A,H52B), C46(H46C,H46D), C47(H47C,H47D),
 C48(H48C,H48D)
;
_shelx_res_checksum              47286
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in oil'
_olex2_submission_original_sample_id 'New BpPtPh2'
_olex2_submission_special_instructions 'No special instructions were received'