1,1-Phosphinoboration of Diazomethanes
Trofimova, Alina; LaFortune, James; Qu, Zheng-wang; Westcott, Stephen; Stephan, Douglas W.; Chemical Communications  (2019) –; doi:10.1039/C9CC06914C

data_7124174
_publ_section_title
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 1,1-Phosphinoboration of Diazomethanes
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06914C
_journal_year                    2019
_chemical_formula_moiety         'C43 H40 B N2 P'
_chemical_formula_sum            'C43 H40 B N2 P'
_chemical_formula_weight         626.61
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2019-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-23 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                94.044(4)
_cell_angle_beta                 94.334(4)
_cell_angle_gamma                96.359(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9419(8)
_cell_length_b                   12.4455(10)
_cell_length_c                   12.8932(9)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.64
_cell_volume                     1734.4(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            65691
_diffrn_reflns_theta_full        28.6988
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.1997
_exptl_crystal_description       shard
_exptl_crystal_F_000             664.4375
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.7103
_refine_diff_density_max         0.4034
_refine_diff_density_min         -0.3426
_refine_diff_density_rms         0.0787
_refine_ls_d_res_high            0.7400
_refine_ls_d_res_low             12.3297
_refine_ls_goodness_of_fit_ref   1.0541
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     430
_refine_ls_number_reflns         8961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0541
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.6021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6595
_reflns_number_total             8961
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc06914c2.cif
_cod_data_source_block           Ph2PBMes2+furanylNN
_cod_database_code               7124174
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C17(H17), C24(H24), C26(H26), C33(H33), C34(H34), C35(H35),
  C36(H36), C39(H39), C40(H40), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C28(H28a,H28b,
 H28c), C29(H29a,H29b,H29c), C30(H30a,H30b,H30c)
;
_olex2_submission_special_instructions 'No special instructions were received'