Ion-bearing stairs: alkali metal complexes of 1,2-diaza-4-phospholides.
Zhao, Minggang; Xue, Tingting; He, Ru-Ru; Ma, Jianping; Zheng, Wenjun; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1634–1645; doi:10.1039/d1dt03601g

data_7709277
_publ_section_title
;
 Ion-bearing stairs: alkali metal complexes of 1,2-diaza-4-phospholides.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1634
_journal_page_last               1645
_journal_paper_doi               10.1039/d1dt03601g
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C10 H18 N2 P S2, 0.5(C24 H48 K2 O12)'
_chemical_formula_sum            'C22 H42 K N2 O6 P S2'
_chemical_formula_weight         564.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-09
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2020-06-01 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2868(5)
_cell_length_b                   13.3235(3)
_cell_length_c                   13.0097(3)
_cell_measurement_reflns_used    2948
_cell_measurement_temperature    230.01(10)
_cell_measurement_theta_max      70.9440
_cell_measurement_theta_min      9.8560
_cell_volume                     2996.40(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      230.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9853
_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    -25.00   1.00   1.00    1.00    --    0.00 122.00 -87.00   26
  2  \w    -19.00  18.00   1.00    1.00    --    0.00  57.00  90.00   37
  3  \w     31.00  65.00   1.00    1.00    --    0.00  57.00  90.00   34
  4  \w     25.00  58.00   1.00    1.00    --   54.00-125.00  30.00   33
  5  \w     26.00  51.00   1.00    1.00    --   54.00-125.00-180.00   25
  6  \w    -19.00  96.00   1.00    1.00    --   54.00   0.00-180.00  115
  7  \w     38.00  74.00   1.00    1.00    --  108.00 -50.00-150.00   36
  8  \w     97.00 127.00   1.00    1.00    --  108.00 -37.00  90.00   30
  9  \w     77.00 136.00   1.00    1.00    --  108.00 -77.00 -30.00   59
 10  \w    105.00 132.00   1.00    1.00    --  108.00 111.00  90.00   27
 11  \w    140.00 177.00   1.00    1.00    --  108.00 111.00  90.00   37
 12  \w     39.00  79.00   1.00    1.00    --  108.00 -37.00  90.00   40
 13  \w    100.00 154.00   1.00    1.00    --  108.00 111.00-180.00   54
 14  \w     40.00 113.00   1.00    1.00    --  108.00-111.00-150.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0601395000
_diffrn_orient_matrix_UB_12      -0.0707181000
_diffrn_orient_matrix_UB_13      -0.0489949000
_diffrn_orient_matrix_UB_21      -0.0403547000
_diffrn_orient_matrix_UB_22      -0.0906788000
_diffrn_orient_matrix_UB_23      0.0500665000
_diffrn_orient_matrix_UB_31      -0.0520294000
_diffrn_orient_matrix_UB_32      -0.0113454000
_diffrn_orient_matrix_UB_33      -0.0954740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7656
_diffrn_reflns_theta_full        70.91
_diffrn_reflns_theta_max         70.92
_diffrn_reflns_theta_min         4.25
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+2.0606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                2542
_reflns_number_total             2981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt03601g2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7709271--7709278.cif.'
_cod_database_code               7709277
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C6 \\sim C8-C6 \\sim C9-C6
 with sigma of 0.01
 C7-C8 \\sim C8-C9 \\sim C9-C7
 with sigma of 0
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C20) = Uanis(C21)
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
 C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) C15(0.5) H15A(0.5)
 H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5) C18(0.5)
 H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 C21(0.5) H21A(0.5) H21B(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) O5(0.5) O6(0.5)
5.a Riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B)
5.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.492
_oxdiff_exptl_absorpt_empirical_full_min 0.806