Addition reactions and diazomethane capture by the intramolecular P-O-B FLP: tBu<sub>2</sub>POBcat.
Zhu, Diya; Qu, Zheng-Wang; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 901–910; doi:10.1039/c9dt04560k

data_7703113
_publ_section_title
;
 Addition reactions and diazomethane capture by the intramolecular P-O-B
 FLP: tBu<sub>2</sub>POBcat.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              901
_journal_page_last               910
_journal_paper_doi               10.1039/c9dt04560k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C27 H32 B N2 O3 P'
_chemical_formula_sum            'C27 H32 B N2 O3 P'
_chemical_formula_weight         474.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-25 deposited with the CCDC.	2019-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                104.696(13)
_cell_angle_beta                 90.64(2)
_cell_angle_gamma                103.469(12)
_cell_formula_units_Z            4
_cell_length_a                   11.168(5)
_cell_length_b                   14.565(7)
_cell_length_c                   16.547(7)
_cell_measurement_reflns_used    4112
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.35
_cell_volume                     2525(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40668
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.690
_diffrn_reflns_theta_min         1.880
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0609 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.9446.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       shard
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         10653
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+1.0551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6106
_reflns_number_total             10653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04560k2.cif
_cod_data_source_block           final_a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7703107--7703116.cif.'
_cod_database_code               7703113
_shelx_shelxl_version_number     2018/3
_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. Rigid bond restraints
 C5, C6, C7, C8
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
4.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C27(H27), C17(H17), C14(H14), C48(H48), C54(H54), C47(H47),
 C23(H23), C44(H44), C21(H21), C46(H46), C40(H40), C50(H50), C25(H25), C13(H13),
  C26(H26), C24(H24), C53(H53), C37(H37), C12(H12), C20(H20), C45(H45),
 C51(H51), C52(H52), C19(H19), C38(H38), C39(H39), C18(H18)
4.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C2(H2A,H2B,H2C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              4766
_olex2_submission_special_instructions 'No special instructions were received'