Facile synthesis of cyclo-(P4tBu3)-containing oligo- and pnictaphosphanes
Eilrich, Volker Jens; Grell, Toni; Lönnecke, Peter; Hey-Hawkins, Evamarie; Dalton Transactions  (2021) –; doi:10.1039/D1DT02639A

data_7708306
_publ_section_title
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 Facile synthesis of cyclo-(P4tBu3)-containing oligo- and pnictaphosphanes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02639A
_journal_year                    2021
_chemical_formula_moiety         'C28 H63 P9'
_chemical_formula_sum            'C28 H63 P9'
_chemical_formula_weight         678.51
_chemical_melting_point          ?
_chemical_name_common            Hepta-tert-butyl-nonaphosphine(7)
_chemical_name_systematic
;
'1,3,3',4,4',5,5'-Hepta-tert-butyl-nonaphosphine(7)'
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
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_audit_update_record
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2021-07-19 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                84.231(2)
_cell_angle_beta                 82.229(2)
_cell_angle_gamma                77.488(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8283(2)
_cell_length_b                   13.4869(3)
_cell_length_c                   15.1621(3)
_cell_measurement_reflns_used    23310
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      35.0270
_cell_measurement_theta_min      2.6660
_cell_volume                     1938.76(7)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.3560
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56616
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.907
_diffrn_reflns_theta_min         2.368
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       plate
_exptl_crystal_F_000             732
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         15838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0275P)^2^+0.3264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13663
_reflns_number_total             15838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02639a2.cif
_cod_data_source_block           x2915
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'Not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7708306
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              57128
_shelx_hkl_checksum              32778