Synthesis of ternary group 13/15 chain compounds.
Köster, Marcel; Kreher, Annikka; von Hänisch, Carsten; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7875–7878; doi:10.1039/c8dt01119b

data_7046442
_publ_section_title
;
 Synthesis of ternary group 13/15 chain compounds.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7875
_journal_page_last               7878
_journal_paper_doi               10.1039/c8dt01119b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C16 H45 B3 N2 P2'
_chemical_formula_sum            'C16 H45 B3 N2 P2'
_chemical_formula_weight         359.91
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.8530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.4536(11)
_cell_length_b                   8.4495(3)
_cell_length_c                   24.1754(10)
_cell_measurement_reflns_used    9356
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.40
_cell_volume                     4821.0(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            165029
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.351
_diffrn_reflns_theta_min         2.405
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.9682.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         12019
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0285P)^2^+3.4485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10062
_reflns_number_total             12019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01119b2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7046442--7046445.cif.'
_cod_database_code               7046442
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-H2 = N1-H1 = N4-H4 = N3-H3
 0.87 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C32(H32A,H32B,H32C), C14(H14A,H14B,H14C), C28(H28A,H28B,
 H28C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C27(H27A,
 H27B,H27C), C30(H30A,H30B,H30C), C16(H16A,H16B,H16C), C7(H7A,H7B,H7C),
 C22(H22A,H22B,H22C), C11(H11A,H11B,H11C), C6(H6D,H6E,H6F), C31(H31A,H31B,H31C),
  C4(H4D,H4E,H4F), C2(H2B,H2C,H2D), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C),
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C3(H3A,H3B,H3C), C20(H20A,H20B,H20C),
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              12940
_olex2_submission_special_instructions 'No special instructions were received'