Diaminophosphinoboranes: effective reagents for phosphinoboration of CO2
Szynkiewicz, Natalia; Ordyszewska, Anna; Chojnacki, Jarosław; Grubba, Rafał; RSC Advances 9 (2019) 27749–; doi:10.1039/C9RA06638A

data_7233622
_publ_section_title
;
 Diaminophosphinoboranes: effective reagents for phosphinoboration of CO2
;
_journal_issue                   48
_journal_name_full               'RSC Advances'
_journal_page_first              27749
_journal_paper_doi               10.1039/C9RA06638A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C22 H42 B N2 P'
_chemical_formula_sum            'C22 H42 B N2 P'
_chemical_formula_weight         376.35
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   fmap
_audit_creation_date             2019-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-29 deposited with the CCDC.    2019-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                91.834(7)
_cell_angle_beta                 92.224(6)
_cell_angle_gamma                97.271(6)
_cell_formula_units_Z            4
_cell_length_a                   9.8205(7)
_cell_length_b                   10.1704(9)
_cell_length_c                   24.3671(19)
_cell_measurement_reflns_used    4716
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      2.22
_cell_volume                     2410.7(3)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction
'X-Area Integrate 1.72.0.0 (STOE, 2018) X-Area LANA 1.71.6.0 (STOE, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0872
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            29277
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.300
_diffrn_reflns_theta_min         2.220
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.9855
_exptl_absorpt_correction_T_min  0.2893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'STOE LANA, absorption correction by scaling of reflection intensities. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different absorption corrections on the model structure of tetrakis(\m~2~-acetato)- diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. Afterwards a spherical absorption correction was performed within STOE LANA.'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         12971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0903P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8086
_reflns_number_total             12971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra06638a2.cif
_cod_data_source_block           2
_cod_database_code               7233622
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.969
_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.a Ternary CH refined with riding coordinates:
 C17(H17), C42(H42), C39(H39), C20(H20), C33(H33), C14(H14), C36(H36), C11(H11)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C2(H2), C28(H28), C24(H24), C26(H26), C6(H6), C5(H5), C27(H27),
 C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C44(H44A,H44B,
 H44C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C19(H19A,
 H19B,H19C), C37(H37A,H37B,H37C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C),
 C43(H43A,H43B,H43C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C),
  C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C15(H15A,H15B,
 H15C), C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C35(H35A,H35B,H35C)
;
_olex2_submission_special_instructions 'No special instructions were received'