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

data_7044385
_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         'C64 H100 Na2 O4 P2'
_chemical_formula_sum            'C64 H100 Na2 O4 P2'
_chemical_formula_weight         1041.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-13
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5335)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7669(6)
_cell_length_b                   16.8927(5)
_cell_length_c                   19.9516(6)
_cell_measurement_reflns_used    7591
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      27.4950
_cell_measurement_theta_min      3.5920
_cell_volume                     6325.1(3)
_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    'ShelXT (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 0.997
_diffrn_measured_fraction_theta_max 0.881
_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    -55.00  28.00   1.00   10.00    --   10.16 -38.00-150.00   83
  2  \w    -19.00  43.00   1.00   10.00    --   10.16 -19.00  60.00   62
  3  \w      4.00  43.00   1.00   10.00    --   10.16 -99.00 -30.00   39
;
_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      -0.0335365000
_diffrn_orient_matrix_UB_12      0.0030141000
_diffrn_orient_matrix_UB_13      -0.0162140000
_diffrn_orient_matrix_UB_21      -0.0022546000
_diffrn_orient_matrix_UB_22      0.0403758000
_diffrn_orient_matrix_UB_23      0.0095116000
_diffrn_orient_matrix_UB_31      0.0172928000
_diffrn_orient_matrix_UB_32      0.0110927000
_diffrn_orient_matrix_UB_33      -0.0301779000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28208
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.773
_diffrn_reflns_theta_min         3.402
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.967
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0505P)^2^+2.1441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4969
_reflns_number_total             7244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02238g2.cif
_cod_data_source_block           3a
_cod_original_cell_volume        6325.2(3)
_cod_database_code               7044385
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C32 H50 Na1 O2 P1'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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
 Na1-O1B \\sim Na1-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim O1B \\sim C29B \\sim C30B
\\sim C31B \\sim C32B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Same fragment restrains
{O1A, C29A, C30A, C31A, C32A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1B, C29B, C30B, C31B, C32B}
5. Others
 Fixed Sof: O1A(0.62679) C29A(0.62679) H29A(0.62679) H29B(0.62679)
 C30A(0.62679) H30A(0.62679) H30B(0.62679) C31A(0.62679) H31A(0.62679)
 H31B(0.62679) C32A(0.62679) H32A(0.62679) H32B(0.62679) O1B(0.37321)
 C29B(0.37321) H29C(0.37321) H29D(0.37321) C30B(0.37321) H30C(0.37321)
 H30D(0.37321) C31B(0.37321) H31C(0.37321) H31D(0.37321) C32B(0.37321)
 H32C(0.37321) H32D(0.37321)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29A(H29A,
 H29B), C30A(H30A,H30B), C31A(H31A,H31B), C32A(H32A,H32B), C29B(H29C,H29D),
 C30B(H30C,H30D), C31B(H31C,H31D), C32B(H32C,H32D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
6.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              83998
_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 1.019
_oxdiff_exptl_absorpt_empirical_full_min 0.981