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

data_7044383
_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         'C40 H66 K O4 P'
_chemical_formula_sum            'C40 H66 K O4 P'
_chemical_formula_weight         680.99
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-13
_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                 91.061(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7963(5)
_cell_length_b                   14.4308(3)
_cell_length_c                   16.6968(5)
_cell_measurement_reflns_used    18381
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.7750
_cell_measurement_theta_min      2.6150
_cell_volume                     4046.34(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   15.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   38.0000 -180.0000 95

  2 omega  -31.00   68.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  -38.0000    0.0000 99

  3 omega   -2.00   87.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905 -125.0000  -60.0000 89

  4 omega   10.00   47.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   28.2599 37

  5 omega   83.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -101.2745 27

  6 omega    9.00   76.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   42.4033 67

  7 omega   22.00   49.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -101.2745 27

  8 omega   64.00  128.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  142.9780 64

  9 omega   16.00  155.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  120.0000 139

 10 omega   20.00   47.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   30.0000 27

 11 omega   22.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -150.0000 52

 12 omega   24.00   76.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   30.0000 52

 13 omega   27.00   66.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   90.0000 39

 14 omega   20.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  150.0000 50

 15 omega   45.00   79.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000   90.0000 34

 16 omega   62.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 30

 17 omega   24.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -60.0000 39

 18 omega   80.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -30.0000 27

 19 omega   12.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000    0.0000 78

 20 omega   93.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000    0.0000 47

 21 omega   23.00   50.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   30.0000 27

 22 omega   80.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   30.0000 41

 23 omega   88.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   42.4033 27

 24 omega   20.00   72.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 52

 25 omega   51.00   82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  120.0000 31

 26 omega   51.00   78.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 27

 27 omega   62.00  123.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -60.0000 61

 28 omega   25.00   52.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000    0.0000 27

 29 omega   63.00   95.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000    0.0000 32

 30 omega   28.00   83.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -90.0000 55

 31 omega   67.00  100.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   28.2599 33

 32 omega  124.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 27

 33 omega   38.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -122.7409 56

 34 omega   86.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 27

 35 omega  125.00  152.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 27

 36 omega   27.00   67.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -30.0000 40

 37 omega   65.00  130.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -34.9578 65

 38 omega   42.00   67.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 25

 39 omega   20.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 54

 40 omega   10.00   35.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -34.9578 25

 41 omega -120.00  -24.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  -77.0000  150.0000 96

 42 omega  -99.00  -18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  125.0000  150.0000 81

 43 omega    8.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000   90.0000 112

 44 omega   12.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   57.0000  -90.0000 104

 45 omega    8.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000    0.0000 112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0004529000
_diffrn_orient_matrix_UB_12      0.0704998000
_diffrn_orient_matrix_UB_13      -0.0693055000
_diffrn_orient_matrix_UB_21      0.0320911000
_diffrn_orient_matrix_UB_22      0.0750327000
_diffrn_orient_matrix_UB_23      0.0577916000
_diffrn_orient_matrix_UB_31      0.0859150000
_diffrn_orient_matrix_UB_32      -0.0282920000
_diffrn_orient_matrix_UB_33      -0.0193478000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56946
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.124
_diffrn_reflns_theta_min         2.631
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.793
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7175
_refine_ls_number_restraints     669
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0847
_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^)+(0.0598P)^2^+9.0929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1995
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6116
_reflns_number_total             7175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02238g2.cif
_cod_data_source_block           4a
_cod_original_cell_volume        4046.36(19)
_cod_database_code               7044383
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C40 H66 O4 P1 K1'
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 K1A-O2A \\sim K1-O2
 with sigma of 0.02
 K1-O4 \\sim K1A-O4A
 with sigma of 0.02
 K1A-P1 \\sim K1-P1
 with sigma of 0.02
 K1-O3 \\sim K1A-O3A
 with sigma of 0.02
 K1-O1 \\sim K1A-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(K1) = Uanis(K1A)
Uanis(O1) = Uanis(O1A)
Uanis(C28) = Uanis(C28A)
Uanis(C27) = Uanis(C27A)
Uanis(C26) = Uanis(C26A)
Uanis(C25) = Uanis(C25A)
Uanis(O3) = Uanis(O3A)
Uanis(C36) = Uanis(C36A)
Uanis(C35) = Uanis(C35A)
Uanis(C34) = Uanis(C34A)
Uanis(C33) = Uanis(C33A)
Uanis(O4) = Uanis(O4A)
Uanis(C37) = Uanis(C37A)
Uanis(C40) = Uanis(C40A)
Uanis(C38) = Uanis(C38A)
Uanis(C39) = Uanis(C39A)
Uanis(O2) = Uanis(O2A)
Uanis(C29) = Uanis(C29A)
Uanis(C30) = Uanis(C30A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
4. Rigid body (RIGU) restrains
 C39A, K1, O1, O2, O3, O4, P1, C39, C38, C37, K1A, O4A, C40A, C37A, C28, C25,
 C29, C32, C33, C36, C40, C11, C1, C13, O1A, O2A, O3A, C38A, C27, C26, C30, C31,
  C34, C35, C10, C2, C6, C14, C18, C28A, C25A, C29A, C32A, C33A, C36A, C26A,
 C12, C3, C7, C5, C15, C19, C17, C22, C27A, C30A, C31A, C34A, C35A, C4, C8, C9,
 C16, C20, C21, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O1A, C28A, C27A, C26A, C25A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1, C28, C27, C26, C25}
{O2A, C29A, C30A, C31A, C32A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O2, C29, C30, C31, C32}
{O3A, C33A, C34A, C35A, C36A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O3, C33, C34, C35, C36}
{O4A, C40A, C39A, C38A, C37A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O4, C40, C39, C38, C37}
6. Others
 Fixed Sof: K1(0.61606) O1(0.61606) C28(0.61606) H28A(0.61606) H28B(0.61606)
 C27(0.61606) H27A(0.61606) H27B(0.61606) C26(0.61606) H26A(0.61606)
 H26B(0.61606) C25(0.61606) H25A(0.61606) H25B(0.61606) O2(0.61606)
 C29(0.61606) H29A(0.61606) H29B(0.61606) C30(0.61606) H30A(0.61606)
 H30B(0.61606) C31(0.61606) H31A(0.61606) H31B(0.61606) C32(0.61606)
 H32A(0.61606) H32B(0.61606) O3(0.61606) C33(0.61606) H33A(0.61606)
 H33B(0.61606) C34(0.61606) H34A(0.61606) H34B(0.61606) C35(0.61606)
 H35A(0.61606) H35B(0.61606) C36(0.61606) H36A(0.61606) H36B(0.61606)
 O4(0.61606) C40(0.61606) H40A(0.61606) H40B(0.61606) C39(0.61606)
 H39A(0.61606) H39B(0.61606) C38(0.61606) H38A(0.61606) H38B(0.61606)
 C37(0.61606) H37A(0.61606) H37B(0.61606) K1A(0.38394) O1A(0.38394)
 C28A(0.38394) H28C(0.38394) H28D(0.38394) C27A(0.38394) H27C(0.38394)
 H27D(0.38394) C26A(0.38394) H26C(0.38394) H26D(0.38394) C25A(0.38394)
 H25C(0.38394) H25D(0.38394) O3A(0.38394) C33A(0.38394) H33C(0.38394)
 H33D(0.38394) C34A(0.38394) H34C(0.38394) H34D(0.38394) C35A(0.38394)
 H35C(0.38394) H35D(0.38394) C36A(0.38394) H36C(0.38394) H36D(0.38394)
 O4A(0.38394) C40A(0.38394) H40C(0.38394) H40D(0.38394) C39A(0.38394)
 H39C(0.38394) H39D(0.38394) C38A(0.38394) H38C(0.38394) H38D(0.38394)
 C37A(0.38394) H37C(0.38394) H37D(0.38394) O2A(0.38394) C29A(0.38394)
 H29C(0.38394) H29D(0.38394) C30A(0.38394) H30C(0.38394) H30D(0.38394)
 C31A(0.38394) H31C(0.38394) H31D(0.38394) C32A(0.38394) H32C(0.38394)
 H32D(0.38394)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
7.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B), C26(H26A,H26B), C25(H25A,H25B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C40(H40A,H40B), C39(H39A,H39B),
  C38(H38A,H38B), C37(H37A,H37B), C28A(H28C,H28D), C27A(H27C,H27D), C26A(H26C,
 H26D), C25A(H25C,H25D), C33A(H33C,H33D), C34A(H34C,H34D), C35A(H35C,H35D),
 C36A(H36C,H36D), C40A(H40C,H40D), C39A(H39C,H39D), C38A(H38C,H38D), C37A(H37C,
 H37D), C29A(H29C,H29D), C30A(H30C,H30D), C31A(H31C,H31D), C32A(H32C,H32D)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
7.d 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), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              18137
_olex2_submission_special_instructions 'No special instructions were received'