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_7703110
_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         'C32 H50 B2 N2 O8 P2'
_chemical_formula_sum            'C32 H50 B2 N2 O8 P2'
_chemical_formula_weight         674.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_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                90
_cell_angle_beta                 98.860(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2242(5)
_cell_length_b                   12.1371(6)
_cell_length_c                   27.8749(13)
_cell_measurement_reflns_used    1884
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.76
_cell_measurement_theta_min      2.24
_cell_volume                     3417.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9973
_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  0.1292
_diffrn_reflns_av_unetI/netI     0.1370
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24213
_diffrn_reflns_theta_full        26.1004
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         1.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0772 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.7940.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3104
_exptl_crystal_description       shard
_exptl_crystal_F_000             1441.5221
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.7930
_refine_diff_density_min         -0.8177
_refine_diff_density_rms         0.1933
_refine_ls_d_res_high            0.8077
_refine_ls_d_res_low             13.7711
_refine_ls_goodness_of_fit_ref   1.0499
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    73
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0499
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                3793
_reflns_number_total             6773
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9dt04560k2.cif
_cod_data_source_block           final_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7703107--7703116.cif.'
_cod_database_code               7703110
_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 Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C20(H20), C21(H21), C15(H15), C16(H16), C23(H23), C14(H14), C22(H22)
2.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C12(H12a,H12b,H12c), C27(H27a,H27b,H27c), C32(H32a,H32b,
 H32c), C26(H26a,H26b,H26c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C10(H10a,H10b,
 H10c), C28(H28a,H28b,H28c), C8(H8a,H8b,H8c), C30(H30a,H30b,H30c), C31(H31a,
 H31b,H31c), C11(H11a,H11b,H11c)
;
_olex2_submission_special_instructions 'No special instructions were received'