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_7709273
_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         'C20 H36 K2 N4 O P2'
_chemical_formula_sum            'C20 H36 K2 N4 O P2'
_chemical_formula_weight         488.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-28
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-24 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                112.772(6)
_cell_angle_beta                 107.548(6)
_cell_angle_gamma                98.919(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3502(6)
_cell_length_b                   12.2677(7)
_cell_length_c                   12.9852(10)
_cell_measurement_reflns_used    3308
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9460
_cell_measurement_theta_min      3.0150
_cell_volume                     1378.53(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0251
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -52.00   42.00   1.0000   11.4150
omega____ theta____ kappa____ phi______ frames
    -       15.6827  -77.0000    0.0000 94

  2 omega   -1.00   83.00   1.0000   11.4150
omega____ theta____ kappa____ phi______ frames
    -       15.6827   57.0000  120.0000 84

  3 omega   35.00   88.00   1.0000   11.4150
omega____ theta____ kappa____ phi______ frames
    -       15.6827  178.0000    0.0000 53

  4 omega   -1.00   83.00   1.0000   11.4150
omega____ theta____ kappa____ phi______ frames
    -       15.6827   57.0000 -180.0000 84

  5 omega  -52.00   32.00   1.0000   11.4150
omega____ theta____ kappa____ phi______ frames
    -       15.6827  -57.0000 -150.0000 84

  6 omega  -25.00   22.00   1.0000   11.4150
omega____ theta____ kappa____ phi______ frames
    -      -17.0890  -99.0000  -60.0000 47

  7 omega   -1.00   32.00   1.0000   11.4150
omega____ theta____ kappa____ phi______ frames
    -       15.6827   57.0000   30.0000 33

  8 omega  -46.00   54.00   1.0000   11.4150
omega____ theta____ kappa____ phi______ frames
    -      -17.0890   19.0000  150.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0341210000
_diffrn_orient_matrix_UB_12      0.0649895000
_diffrn_orient_matrix_UB_13      0.0356854000
_diffrn_orient_matrix_UB_21      -0.0098127000
_diffrn_orient_matrix_UB_22      0.0061972000
_diffrn_orient_matrix_UB_23      -0.0537026000
_diffrn_orient_matrix_UB_31      -0.0667165000
_diffrn_orient_matrix_UB_32      0.0092406000
_diffrn_orient_matrix_UB_33      -0.0028663000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16722
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.340
_diffrn_reflns_theta_min         3.022
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5628
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.1183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3643
_reflns_number_total             5628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03601g2.cif
_cod_data_source_block           150114-1a
_cod_depositor_comments
'Adding full bibliography for 7709271--7709278.cif.'
_cod_original_cell_volume        1378.53(17)
_cod_database_code               7709273
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.898
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
C6 \\sim C7 \\sim C8: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C14(H14), C3(H3), C11(H11), C6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C17(H17a,H17b), C18(H18a,H18b), C19(H19a,H19b)
3.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C7(H7a,H7b,H7c), C15(H15a,H15b,H15c), C10(H10a,H10b,H10c),
 C1(H1a,H1b,H1c), C16(H16a,H16b,H16c), C9(H9a,H9b,H9c), C2(H2a,H2b,H2c)
;
_shelx_res_checksum              43297
_shelx_hkl_checksum              4345
_olex2_submission_special_instructions 'No special instructions were received'