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_7046445
_publ_section_title
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 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         'C20 H47 Ga N P, 0.5(C6 H6)'
_chemical_formula_sum            'C23 H50 Ga N P'
_chemical_formula_weight         441.33
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                71.092(2)
_cell_angle_beta                 85.633(3)
_cell_angle_gamma                70.883(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7135(5)
_cell_length_b                   11.0101(6)
_cell_length_c                   15.2569(8)
_cell_measurement_reflns_used    9051
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.421
_cell_measurement_theta_min      2.667
_cell_volume                     1307.61(13)
_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                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50635
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.432
_diffrn_reflns_theta_min         2.475
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1150 before and 0.0377 after correction. The Ratio of minimum to maximum transmission is 0.8390. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.529
_exptl_crystal_size_mid          0.485
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.4480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5201
_reflns_number_total             5365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01119b2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7046442--7046445.cif.'
_cod_database_code               7046445
_shelx_shelxl_version_number     2014/7
_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. Others
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=1-FVAR(2)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(3)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(3)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(4)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(4)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=1-FVAR(5)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(5)
3.a Aromatic/amide H refined with riding coordinates:
 C80(H80), C82(H82), C81(H81)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C5(H5A,
 H5B,H5C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,
 H14B,H14C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C),
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C25(H25A,
 H25B,H25C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C),
 C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'