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

data_7044386
_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         'C36 H58 Li O3 P, C36.02 H58.62 Li O3.01 P'
_chemical_formula_sum            'C72.02 H116.62 Li2 O6.01 P2'
_chemical_formula_weight         1154.41
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-24
_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                68.346(3)
_cell_angle_beta                 80.5527(18)
_cell_angle_gamma                89.5652(18)
_cell_formula_units_Z            2
_cell_length_a                   11.32606(19)
_cell_length_b                   17.4145(5)
_cell_length_c                   19.3933(5)
_cell_measurement_reflns_used    22496
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.8490
_cell_measurement_theta_min      3.9560
_cell_volume                     3501.07(17)
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   13.00  113.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   57.0000  -60.0000 100

  2 omega  -25.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155  -57.0000  150.0000 94

  3 omega   -1.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155 -125.0000   90.0000 72

  4 omega   36.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   38.0000 -120.0000 26

  5 omega   11.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -171.9710 95

  6 omega   18.00  133.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   30.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -60.3306 44

  8 omega   49.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  120.0000 28

  9 omega   97.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   59.3439 26

 10 omega   87.00  151.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -90.0000 64

 11 omega  143.00  168.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000 -150.0000 25

 12 omega  108.00  164.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000 -150.0000 56

 13 omega   66.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -90.0000 25

 14 omega  122.00  167.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -90.0000 45

 15 omega   24.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   30.0000 46

 16 omega   58.00  107.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  122.4333 49

 17 omega   21.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 55

 18 omega   12.00   38.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -90.0000 26

 19 omega   51.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -90.0000 32

 20 omega   23.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -30.0000 34

 21 omega   26.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 49

 22 omega   83.00  120.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000 -150.0000 37

 23 omega   98.00  177.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000    0.0000 79

 24 omega   77.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000 -150.0000 26

 25 omega   36.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000    0.0000 26

 26 omega  119.00  145.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000   90.0000 26

 27 omega   20.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000    0.0000 48

 28 omega   31.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -90.0000 37

 29 omega   51.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000   30.0000 32

 30 omega   22.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -150.0000 55

 31 omega    9.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  122.4333 30

 32 omega   87.00  130.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -60.3306 43

 33 omega   34.00   60.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   30.0000 26

 34 omega   46.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -90.0000 42

 35 omega    9.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -180.0000 46

 36 omega   78.00  104.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -180.0000 26

 37 omega   62.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 26

 38 omega   98.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 25

 39 omega   14.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 43

 40 omega   24.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000 -180.0000 25

 41 omega   96.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000    4.5345 27

 42 omega   39.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000    4.5345 36

 43 omega  -71.00   25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7155   57.0000  -30.0000 96

 44 omega    8.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   77.0000 -180.0000 112

 45 omega    8.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   77.0000   30.0000 112

 46 omega   12.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   57.0000  120.0000 104
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0013714000
_diffrn_orient_matrix_UB_12      0.0772535000
_diffrn_orient_matrix_UB_13      -0.0721901000
_diffrn_orient_matrix_UB_21      -0.0156316000
_diffrn_orient_matrix_UB_22      -0.0558501000
_diffrn_orient_matrix_UB_23      -0.0440667000
_diffrn_orient_matrix_UB_31      -0.1372260000
_diffrn_orient_matrix_UB_32      0.0015887000
_diffrn_orient_matrix_UB_33      0.0194624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49842
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.966
_diffrn_reflns_theta_min         2.489
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95066
_exptl_absorpt_correction_type   multi-scan
_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)
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    1.095
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1266
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         12397
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0522P)^2^+0.7854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9868
_reflns_number_total             12397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02238g2.cif
_cod_data_source_block           2a
_cod_original_cell_volume        3501.06(16)
_cod_database_code               7044386
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C72 H102 P3 As1'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6C-C69C \\sim O6C-C71C
 with sigma of 0.02
 C36-C35B \\sim C35A-C36
 with sigma of 0.02
 C35A-C34 \\sim C34-C35B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C71A \\sim C72A \\sim C71C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O6A \\sim O6B \\sim O6C: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C69A \\sim C69B \\sim C69C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C71A \\sim C71C: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C71A \\sim C71B \\sim C72C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C70A \\sim C70B \\sim C70C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C35A \\sim C35B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Rigid body (RIGU) restrains
 O6A, C69A, C70A, C71A, C71A, C72A, O6B, C69B, C70B, C71B, O6C, C69C, C70C,
 C71C, C72C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O6A, C69A, C70A, C71A, C72A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O6B, C69B, C70B, C71B, C72B}
6. Others
 Fixed Sof: H34A(0.72735) H34B(0.72735) H34C(0.27265) H34D(0.27265)
 H36A(0.72735) H36B(0.72735) H36C(0.27265) H36D(0.27265) O6A(0.39127)
 C69A(0.39127) H69A(0.39127) H69B(0.39127) C70A(0.39127) H70A(0.39127)
 H70B(0.39127) C71A(0.39127) H71A(0.39127) H71B(0.39127) C72A(0.39127)
 H72A(0.39127) H72B(0.39127) C35A(0.72735) H35A(0.72735) H35B(0.72735)
 O6B(0.32268) C69B(0.32268) H69C(0.32268) H69D(0.32268) C70B(0.32268)
 H70C(0.32268) H70D(0.32268) C71B(0.32268) H71C(0.32268) H71D(0.32268)
 C72B(0.32268) H72C(0.32268) H72D(0.32268) C35B(0.27265) H35C(0.27265)
 H35D(0.27265) O6C(0.2913) C69C(0.2913) H69E(0.2913) H69F(0.2913) C70C(0.2913)
 H70E(0.2913) H70F(0.2913) H70G(0.2913) C71C(0.2913) H71E(0.2913) H71F(0.2913)
 C72C(0.2913) H72E(0.2913) H72F(0.2913) H72G(0.2913)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C43(H43), C46(H46), C55(H55), C58(H58)
7.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C34(H34C,H34D), C36(H36A,H36B), C36(H36C,H36D), C61(H61A,H61B),
  C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,
 H66B), C67(H67A,H67B), C68(H68A,H68B), C69A(H69A,H69B), C70A(H70A,H70B),
 C71A(H71A,H71B), C72A(H72A,H72B), C35A(H35A,H35B), C69B(H69C,H69D), C70B(H70C,
 H70D), C71B(H71C,H71D), C72B(H72C,H72D), C35B(H35C,H35D), C69C(H69E,H69F),
 C71C(H71E,H71F)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C39(H39), C40(H40),
 C41(H41), C51(H51), C52(H52), C53(H53)
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), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C70C(H70E,H70F,H70G), C72C(H72E,H72F,H72G)
;
_shelx_res_checksum              37945
_olex2_submission_special_instructions 'No special instructions were received'