Desolvation and aggregation of sterically demanding alkali metal diarylphosphides
Izod, Keith; Evans, Peter; Waddell, Paul G.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02238G

data_7044382
_publ_section_title
;
 Desolvation and aggregation of sterically demanding alkali metal
 diarylphosphides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02238G
_journal_year                    2017
_chemical_formula_moiety         'C24 H35 P'
_chemical_formula_sum            'C24 H35 P'
_chemical_formula_weight         354.49
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1101(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.75472(8)
_cell_length_b                   19.0684(2)
_cell_length_c                   14.79343(17)
_cell_measurement_reflns_used    14016
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.6290
_cell_measurement_theta_min      3.7640
_cell_volume                     2187.50(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -86.00  -48.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  138.0000  -48.0000 38

  2 omega   69.00  116.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  131.0000  136.0000 47

  3 omega   14.00  106.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   57.0000 -120.0000 92

  4 omega   51.00   85.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905 -138.0000 -109.0000 34

  5 omega   15.00  113.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   38.0000  150.0000 98

  6 omega   60.00  132.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -110.4725 72

  7 omega   78.00  118.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   -2.8723 40

  8 omega   15.00   41.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  167.1857 26

  9 omega   51.00  118.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -120.0000 67

 10 omega   21.00   77.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 56

 11 omega   25.00   75.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 50

 12 omega  106.00  165.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000    0.0000 59

 13 omega   65.00   95.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  -90.0000 30

 14 omega   38.00   67.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -30.0000 29

 15 omega   10.00   41.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   -2.8723 31

 16 omega   51.00  103.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   90.0000 52

 17 omega   57.00   87.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   90.0000 30

 18 omega   43.00   68.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -30.0000 25

 19 omega   26.00   51.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   90.0000 25

 20 omega   21.00   57.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 36

 21 omega   23.00   49.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   60.0000 26

 22 omega   29.00   72.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000 -150.0000 43

 23 omega   17.00   82.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  150.0000 65

 24 omega   71.00   97.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000    0.0000 26

 25 omega   55.00  175.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -60.0000 120

 26 omega   80.00  107.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  167.1857 27

 27 omega   87.00  123.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  107.4598 36

 28 omega   15.00   41.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 26

 29 omega   42.00   68.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 26

 30 omega  103.00  141.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000 -180.0000 38

 31 omega   47.00   74.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 27

 32 omega   48.00   77.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  120.0000 29

 33 omega   52.00   96.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  150.0000 44

 34 omega   10.00   59.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  107.4598 49

 35 omega    8.00  120.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000    0.0000 112

 36 omega   65.00  115.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  138.0000  -48.0000 50

 37 omega    8.00  120.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000  -90.0000 112

 38 omega    8.00  120.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000 -180.0000 112

 39 omega    8.00  120.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000   90.0000 112

 40 omega   66.00  168.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -180.0000 102

 41 omega   66.00  168.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   90.0000 102

 42 omega   63.00  145.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000   30.0000 82
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1915362000
_diffrn_orient_matrix_UB_12      0.0153843000
_diffrn_orient_matrix_UB_13      -0.0191953000
_diffrn_orient_matrix_UB_21      0.0360488000
_diffrn_orient_matrix_UB_22      -0.0792880000
_diffrn_orient_matrix_UB_23      -0.0065862000
_diffrn_orient_matrix_UB_31      -0.0386268000
_diffrn_orient_matrix_UB_32      0.0021732000
_diffrn_orient_matrix_UB_33      -0.1021205000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31461
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.936
_diffrn_reflns_theta_min         2.317
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3874
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.4735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3578
_reflns_number_total             3874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02238g2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2187.51(4)
_cod_database_code               7044382
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C24 H35 P1'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8158(11) 0.1842(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C23B-C22 \\sim C23A-C22
 with sigma of 0.02
 C24B-C22 \\sim C24A-C22
 with sigma of 0.02
 C24A-C23A \\sim C24B-C23B
 with sigma of 0.02
 P1-H1B \\sim P1-H1A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C23B) = Uanis(C23A)
Uanis(C24B) = Uanis(C24A)
5. Others
 Fixed Sof: H1A(0.52006) H1B(0.47994) H22(0.52006) H22A(0.47994) C23A(0.52006)
 H23A(0.52006) H23B(0.52006) H23C(0.52006) C24A(0.52006) H24A(0.52006)
 H24B(0.52006) H24C(0.52006) C23B(0.47994) H23D(0.47994) H23E(0.47994)
 H23F(0.47994) C24B(0.47994) H24D(0.47994) H24E(0.47994) H24F(0.47994)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C22(H22A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23A(H23A,H23B,H23C), C24A(H24A,H24B,
 H24C), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F)
;
_shelx_res_checksum              67150
_olex2_submission_special_instructions 'No special instructions were received'