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_7703107
_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         'C24 H33 B N O4 P, C H2 Cl2'
_chemical_formula_sum            'C25 H35 B Cl2 N O4 P'
_chemical_formula_weight         526.26
_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
_audit_creation_date             2019-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-02 deposited with the CCDC.	2019-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                83.507(5)
_cell_angle_beta                 85.826(4)
_cell_angle_gamma                81.688(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4602(8)
_cell_length_b                   8.5103(9)
_cell_length_c                   18.4139(19)
_cell_measurement_reflns_used    3769
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.23
_cell_volume                     1301.3(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 0.9979
_diffrn_measured_fraction_theta_max 0.9979
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19957
_diffrn_reflns_theta_full        26.0169
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1562 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.9192.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3430
_exptl_crystal_description       plate
_exptl_crystal_F_000             557.0252
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.6215
_refine_diff_density_min         -0.5539
_refine_diff_density_rms         0.1220
_refine_ls_d_res_high            0.8102
_refine_ls_d_res_low             7.7704
_refine_ls_goodness_of_fit_ref   1.0323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    51
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0323
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.5764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3584
_reflns_number_total             5124
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9dt04560k2.cif
_cod_data_source_block           FINAL_a
_cod_depositor_comments
'Adding full bibliography for 7703107--7703116.cif.'
_cod_database_code               7703107
_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.a Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C19(H19), C22(H22), C13(H13), C14(H14)
2.c Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C7(H7a,H7b,H7c), C18(H18a,H18b,H18c), C9(H9a,H9b,H9c),
 C24(H24a,H24b,H24c), C4(H4a,H4b,H4c), C8(H8a,H8b,H8c), C5(H5a,H5b,H5c),
 C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'