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_7709276
_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 Se2, 0.5(C24 H48 K2 O12)'
_chemical_formula_sum            'C22 H42 K N2 O6 P Se2'
_chemical_formula_weight         658.57
_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             2020-11-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2021-03-31 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                   17.1551(9)
_cell_length_b                   13.4665(7)
_cell_length_c                   13.0108(6)
_cell_measurement_reflns_used    4638
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.8670
_cell_measurement_theta_min      8.4530
_cell_volume                     3005.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9768
_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      7.00  41.00   1.00    1.00    --   54.00 -98.00 -61.00   34
  2  \w     34.00  61.00   1.00    1.00    --   54.00 -75.00-175.00   27
  3  \w      0.00  33.00   1.00    1.00    --   54.00 -54.00  33.00   33
  4  \w     69.00  95.00   1.00    1.00    --   54.00 -98.00 -61.00   26
  5  \w    128.00 155.00   1.00    1.00    --  108.00  75.00 -47.00   27
  6  \w     87.00 112.00   1.00    1.00    --  108.00 -75.00-175.00   25
  7  \w     44.00 100.00   1.00    1.00    --  108.00 -98.00 -61.00   56
  8  \w     53.00  98.00   1.00    1.00    --  108.00 -54.00  33.00   45
  9  \w    -19.00  29.00   1.00    1.00    --    0.00 -77.00   0.00   48
 10  \w    -20.00  25.00   1.00    1.00    --    0.00 -77.00 150.00   45
 11  \w     34.00 120.00   1.00    1.00    --   54.00  57.00-150.00   86
 12  \w     75.00 111.00   1.00    1.00    --   54.00-125.00-120.00   36
 13  \w    103.00 178.00   1.00    1.00    --  108.00  77.00 -90.00   75
 14  \w     37.00 103.00   1.00    1.00    --  108.00 -91.00-180.00   66
 15  \w     38.00  95.00   1.00    1.00    --  108.00 -91.00  60.00   57
 16  \w    110.00 136.00   1.00    1.00    --  108.00  98.00  45.00   26
;
_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      0.0265410000
_diffrn_orient_matrix_UB_12      -0.1071404000
_diffrn_orient_matrix_UB_13      0.0212927000
_diffrn_orient_matrix_UB_21      0.0689464000
_diffrn_orient_matrix_UB_22      0.0143372000
_diffrn_orient_matrix_UB_23      -0.0745069000
_diffrn_orient_matrix_UB_31      0.0509706000
_diffrn_orient_matrix_UB_32      0.0373023000
_diffrn_orient_matrix_UB_33      0.0896800000
_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  0.0711
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7954
_diffrn_reflns_theta_full        67.06
_diffrn_reflns_theta_max         67.07
_diffrn_reflns_theta_min         4.26
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.118
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.249
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2807
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.1088
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+111.0268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2542
_refine_ls_wR_factor_ref         0.2558
_reflns_number_gt                2659
_reflns_number_total             2807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt03601g2.cif
_cod_data_source_block           exp_26
_cod_depositor_comments
'Adding full bibliography for 7709271--7709278.cif.'
_cod_database_code               7709276
_diffrn_oxdiff_digest_frames
;
01d536b101ac5ed609e437839be6fdd63e00028e9c5
;
_diffrn_oxdiff_digest_hkl
;
01fd337345e5abf903e9ea0c9cb80779f9491b
;
_reflns_odcompleteness_completeness 99.84
_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
 C8-C6 = C9A-C6
 1.53 with sigma of 0.01
 O1-C19 = O2-C20 = O6-C22 = O1-C21
 1.36 with sigma of 0.01
 O2-C9 = O3-C10 = O3-C11 = O4-C12 = O4-C13 = O5-C14 = O5-C15 = O6-C16
 1.36 with sigma of 0.01
 C9-C10 = C11-C12 = C13-C14 = C15-C16 = C19-C20 = C21-C22
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C11(0.5) H11A(0.5) H11B(0.5) O1(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) C19(0.5) H19A(0.5) H19B(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 O3(0.5) O2(0.5) C10(0.5) H10A(0.5) H10B(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 O5(0.5) O4(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 C14(0.5) H14A(0.5) H14B(0.5) C21(0.5) H21A(0.5) H21B(0.5) O6(0.5) C20(0.5)
 H20A(0.5) H20B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C6(0.5) H7A(0.5) H7B(0.5)
 H7C(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5)
 H9AC(0.5)
5.a Riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B), C19(H19A,H19B), C12(H12A,H12B), C10(H10A,H10B),
 C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C14(H14A,H14B), C21(H21A,H21B),
  C20(H20A,H20B), C22(H22A,H22B), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9A(H9AA,
 H9AB,H9AC)
5.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C1(H1A,H1B,H1C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.691