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

data_7044381
_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         'C33 H52 Li O3 P'
_chemical_formula_sum            'C33 H52 Li O3 P'
_chemical_formula_weight         534.65
_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             2016-04-27
_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                82.213(4)
_cell_angle_beta                 89.691(4)
_cell_angle_gamma                65.484(5)
_cell_formula_units_Z            2
_cell_length_a                   9.5265(4)
_cell_length_b                   9.5469(5)
_cell_length_c                   19.4340(10)
_cell_measurement_reflns_used    4999
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.4700
_cell_measurement_theta_min      4.5710
_cell_volume                     1590.78(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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      air
_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 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -99.00 -18.00   1.00    4.00    --  -41.59 125.00-150.00   81
  2  \w    -40.00  88.00   1.00    4.00    --   41.59 -19.00   0.00  128
  3  \w     15.00 117.00   1.00    4.00    --   41.59  38.00-180.00  102
  4  \w     -3.00  96.00   1.00    4.00    --   41.59-125.00 -60.00   99
  5  \w      9.00 133.00   1.00   16.00    --   93.50 -93.00-168.95  124
  6  \w      9.00 133.00   1.00   16.00    --   93.50 -93.00  23.20  124
  7  \w      9.00 133.00   1.00   16.00    --   93.50 -93.00  72.15  124
  8  \w      9.00 133.00   1.00   16.00    --   93.50 -92.00-141.57  124
  9  \w      9.00 133.00   1.00   16.00    --   93.50 -93.00 -52.40  124
 10  \w     63.00 168.00   1.00   16.00    --   93.50  61.00  60.00  105
 11  \w     66.00 168.00   1.00   16.00    --   93.50  45.00 -30.00  102
 12  \w      9.00  83.00   1.00   16.00    --   93.50 -94.00 -30.00   74
 13  \w     32.00 174.00   1.00   16.00    --   93.50  15.00  90.00  142
 14  \w     64.00 140.00   1.00   16.00    --   93.50  61.00 120.00   76
 15  \w     18.00 100.00   1.00   16.00    --   93.50 -90.00 134.38   82
 16  \w    120.00 167.00   1.00   16.00    --   93.50 125.00   0.00   47
 17  \w     67.00 168.00   1.00   16.00    --   93.50  61.00   0.00  101
 18  \w     68.00 135.00   1.00   16.00    --   93.50  77.00 -90.00   67
 19  \w    118.00 169.00   1.00   16.00    --   93.50  69.00  35.35   51
 20  \w     46.00 123.00   1.00   16.00    --   93.50 -30.00 -30.00   77
 21  \w      9.00  41.00   1.00   16.00    --   93.50 -94.00   0.00   32
 22  \w     48.00  73.00   1.00   16.00    --   93.50 -94.00   0.00   25
 23  \w    110.00 147.00   1.00   16.00    --   93.50 125.00 -90.00   37
 24  \w     10.00  68.00   1.00   16.00    --   93.50 -94.00-150.00   58
 25  \w    116.00 158.00   1.00   16.00    --   93.50 125.00 150.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0840968000
_diffrn_orient_matrix_UB_12      -0.1741949000
_diffrn_orient_matrix_UB_13      -0.0064851000
_diffrn_orient_matrix_UB_21      -0.0387267000
_diffrn_orient_matrix_UB_22      -0.0423897000
_diffrn_orient_matrix_UB_23      0.0748300000
_diffrn_orient_matrix_UB_31      -0.1520518000
_diffrn_orient_matrix_UB_32      0.0022150000
_diffrn_orient_matrix_UB_33      -0.0279355000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22353
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.058
_diffrn_reflns_theta_min         4.600
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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    1.116
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0592P)^2^+0.4357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4366
_reflns_number_total             5634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02238g2.cif
_cod_data_source_block           7a
_cod_original_cell_volume        1590.76(15)
_cod_database_code               7044381
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C21 H28 Li1 P1'
_reflns_odcompleteness_completeness 99.70
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), 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)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C17(H17)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              31478
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.046
_oxdiff_exptl_absorpt_empirical_full_min 0.741