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_7124173
_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 H42 B N2 P, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C43.5 H43 B Cl N2 P'
_chemical_formula_weight         671.09
_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                95.608(6)
_cell_angle_beta                 107.365(6)
_cell_angle_gamma                97.228(6)
_cell_formula_units_Z            2
_cell_length_a                   11.4929(15)
_cell_length_b                   12.5079(14)
_cell_length_c                   13.5474(17)
_cell_measurement_reflns_used    5383
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      2.30
_cell_volume                     1825.0(4)
_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 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_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  0.0860
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43911
_diffrn_reflns_theta_full        28.2818
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2211
_exptl_crystal_description       block
_exptl_crystal_F_000             710.7386
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.6878
_refine_diff_density_max         1.0493
_refine_diff_density_min         -0.9119
_refine_diff_density_rms         0.1232
_refine_ls_d_res_high            0.7500
_refine_ls_d_res_low             12.7973
_refine_ls_goodness_of_fit_ref   1.0275
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    75
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0275
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+0.8972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5343
_reflns_number_total             9041
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc06914c2.cif
_cod_data_source_block           Ph2PBMes2+Ph2CNN
_cod_database_code               7124173
_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. Others
 Fixed Sof: C1S(0.5) H1Sa(0.5) H1Sb(0.5) Cl1S(0.5) Cl2S(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1S(H1Sa,H1Sb)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C28(H28), C30(H30), C37(H37), C39(H39)
3.c Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c), C41(H41a,H41b,
 H41c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c)
;
_olex2_submission_special_instructions 'No special instructions were received'