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_7709272
_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         'C36 H36 K2 N4 O2 P2'
_chemical_formula_sum            'C36 H36 K2 N4 O2 P2'
_chemical_formula_weight         696.83
_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             2021-04-29
_audit_creation_method
;
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                112.737(4)
_cell_angle_beta                 108.856(4)
_cell_angle_gamma                101.438(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4944(5)
_cell_length_b                   12.9078(6)
_cell_length_c                   13.8901(6)
_cell_measurement_reflns_used    4621
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2450
_cell_measurement_theta_min      3.0760
_cell_volume                     1816.16(18)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -11.00   83.00   1.0000   10.3600
omega____ theta____ kappa____ phi______ frames
    -       15.6827   77.0000  150.0000 94

  2 omega  -52.00   42.00   1.0000   10.3600
omega____ theta____ kappa____ phi______ frames
    -       15.6827  -77.0000   30.0000 94

  3 omega   -1.00   83.00   1.0000   10.3600
omega____ theta____ kappa____ phi______ frames
    -       15.6827   57.0000   30.0000 84

  4 omega  -54.00   35.00   1.0000   10.3600
omega____ theta____ kappa____ phi______ frames
    -       15.6827  -37.0000 -120.0000 89

  5 omega  -44.00   50.00   1.0000   10.3600
omega____ theta____ kappa____ phi______ frames
    -      -17.0890   77.0000 -120.0000 94

  6 omega  -25.00   22.00   1.0000   10.3600
omega____ theta____ kappa____ phi______ frames
    -      -17.0890  -99.0000   30.0000 47

  7 omega  -36.00   46.00   1.0000   10.3600
omega____ theta____ kappa____ phi______ frames
    -      -17.0890   37.0000  150.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0453362000
_diffrn_orient_matrix_UB_12      0.0214557000
_diffrn_orient_matrix_UB_13      0.0570210000
_diffrn_orient_matrix_UB_21      0.0384809000
_diffrn_orient_matrix_UB_22      0.0426324000
_diffrn_orient_matrix_UB_23      -0.0064559000
_diffrn_orient_matrix_UB_31      -0.0251873000
_diffrn_orient_matrix_UB_32      0.0428514000
_diffrn_orient_matrix_UB_33      0.0227622000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22239
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.343
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69828
_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    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0760P)^2^+0.4230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4737
_reflns_number_total             7433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03601g2.cif
_cod_data_source_block           141224-1o
_cod_depositor_comments
'Adding full bibliography for 7709271--7709278.cif.'
_cod_original_cell_volume        1816.17(16)
_cod_database_code               7709272
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.920
_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
2.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C34(H34A,H34B), C33(H33A,H33B), C32(H32A,
 H32B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C27(H27), C12(H12), C11(H11), C4(H4), C5(H5), C10(H10),
 C25(H25), C19(H19), C26(H26), C18(H18), C3(H3), C2(H2), C28(H28), C24(H24),
 C1(H1), C13(H13), C15(H15), C14(H14)
;
_shelx_res_checksum              32955
_shelx_hkl_checksum              46093
_olex2_submission_special_instructions 'No special instructions were received'