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_7703108
_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         'C28 H30 B O5 P, C H2 Cl2'
_chemical_formula_sum            'C29 H32 B Cl2 O5 P'
_chemical_formula_weight         573.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_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                90
_cell_angle_beta                 93.502(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4123(12)
_cell_length_b                   23.192(3)
_cell_length_c                   14.1688(16)
_cell_measurement_reflns_used    2342
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.58
_cell_measurement_theta_min      2.58
_cell_volume                     2759.1(6)
_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 0.9975
_diffrn_measured_fraction_theta_max 0.9975
_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  0.0907
_diffrn_reflns_av_unetI/netI     0.1078
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19845
_diffrn_reflns_theta_full        25.6804
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.3799
_exptl_crystal_description       shard
_exptl_crystal_F_000             1202.1330
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.9383
_refine_diff_density_min         -1.5629
_refine_diff_density_rms         0.1765
_refine_ls_d_res_high            0.8200
_refine_ls_d_res_low             8.9670
_refine_ls_goodness_of_fit_ref   1.0494
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    51
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0494
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1082P)^2^+4.9001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1971
_refine_ls_wR_factor_ref         0.2358
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -10
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              -7
_reflns_number_gt                2997
_reflns_number_total             5226
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9dt04560k2.cif
_cod_data_source_block           FINAL_a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7703107--7703116.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7703108
_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:
 C29(H29a,H29b)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C24(H24), C25(H25), C14(H14), C12(H12), C13(H13), C4(H4), C7(H7),
 C26(H26), C27(H27), C6(H6), C5(H5)
2.c Idealised Me refined as rotating group:
 C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C16(H16a,H16b,H16c), C18(H18a,H18b,
 H18c), C22(H22a,H22b,H22c), C17(H17a,H17b,H17c)
;
_olex2_submission_special_instructions 'No special instructions were received'