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

data_7044379
_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         'C48 H70 Li2 O3 P2'
_chemical_formula_sum            'C48 H70 Li2 O3 P2'
_chemical_formula_weight         770.86
_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             2016-03-30
_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                 102.271(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0982(2)
_cell_length_b                   15.7006(3)
_cell_length_c                   24.9514(6)
_cell_measurement_reflns_used    7258
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.5870
_cell_measurement_theta_min      3.2930
_cell_volume                     4631.21(17)
_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      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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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     12.00 116.00   1.00   10.00    --   41.59  57.00-150.00  104
  2  \w     15.00 117.00   1.00   10.00    --   41.59  38.00 -30.00  102
  3  \w     -3.00  96.00   1.00   10.00    --   41.59-125.00-180.00   99
  4  \w      9.00 133.00   1.00   40.00    --   93.50 -92.00  42.36  124
  5  \w     29.00  82.00   1.00   40.00    --   93.50 -94.00 -30.00   53
  6  \w     24.00  63.00   1.00   40.00    --   93.50 -30.00 -60.00   39
  7  \w     70.00 124.00   1.00   40.00    --   93.50 -92.00 105.03   54
  8  \w     12.00  38.00   1.00   40.00    --   93.50 -94.00 -60.00   26
  9  \w     54.00  80.00   1.00   40.00    --   93.50 -94.00 -60.00   26
 10  \w     49.00  95.00   1.00   40.00    --   93.50-125.00 120.00   46
 11  \w     29.00  66.00   1.00   40.00    --   93.50 -94.00 -90.00   37
 12  \w     88.00 114.00   1.00   40.00    --   93.50 -30.00 -60.00   26
 13  \w     10.00  82.00   1.00   40.00    --   93.50 -94.00 150.00   72
 14  \w     64.00 170.00   1.00   40.00    --   93.50  30.00-120.00  106
 15  \w     23.00  58.00   1.00   40.00    --   93.50 -92.00 105.03   35
 16  \w     27.00  72.00   1.00   40.00    --   93.50 -45.00 120.00   45
 17  \w     86.00 121.00   1.00   40.00    --   93.50 -45.00 120.00   35
 18  \w     46.00  72.00   1.00   40.00    --   93.50  15.00 -30.00   26
 19  \w    122.00 152.00   1.00   40.00    --   93.50  15.00 -30.00   30
 20  \w     50.00 128.00   1.00   40.00    --   93.50 -93.00 179.27   78
;
_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      -0.0152333000
_diffrn_orient_matrix_UB_12      -0.0974509000
_diffrn_orient_matrix_UB_13      -0.0003497000
_diffrn_orient_matrix_UB_21      -0.0577001000
_diffrn_orient_matrix_UB_22      0.0033611000
_diffrn_orient_matrix_UB_23      -0.0612840000
_diffrn_orient_matrix_UB_31      0.1157980000
_diffrn_orient_matrix_UB_32      -0.0111601000
_diffrn_orient_matrix_UB_33      -0.0154364000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33402
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.944
_diffrn_reflns_theta_min         3.348
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8211
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0499P)^2^+0.5205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6035
_reflns_number_total             8211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02238g2.cif
_cod_data_source_block           8a
_cod_database_code               7044379
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C48 H70 Li2 O3 P2'
_reflns_odcompleteness_completeness 99.82
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C39B-C38 \\sim C39A-C38
 with sigma of 0.02
 C40-C39B \\sim C40-C39A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C39A) = Uanis(C39B)
4. Others
 Sof(H8BD)=Sof(H8BE)=Sof(H8BF)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=FVAR(1)
 Fixed Sof: H38A(0.81767) H38B(0.81767) H38C(0.18233) H38D(0.18233)
 C39A(0.81767) H39A(0.81767) H39B(0.81767) C39B(0.18233) H39C(0.18233)
 H39D(0.18233) H40A(0.81767) H40B(0.81767) H40C(0.18233) H40D(0.18233)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C38(H38C,H38D), C39A(H39A,H39B), C39B(H39C,
 H39D), C40(H40A,H40B), C40(H40C,H40D), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,H47B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23), C30(H30), C32(H32)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8AA,H8AB,H8AC), C8(H8BD,H8BE,H8BF), C9(H9A,H9B,H9C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              6652
_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 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.747