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_7709271
_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 K N2 P'
_chemical_formula_sum            'C10 H18 K N2 P'
_chemical_formula_weight         236.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-09-21
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Olex2 1.2
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2020-06-01 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90.804(6)
_cell_angle_gamma                90
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_cell_length_c                   20.6520(11)
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_cell_measurement_theta_min      3.5520
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
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_diffrn_ambient_temperature      293(2)
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
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  1 omega  -11.00   83.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       15.6827   77.0000   60.0000 94

  2 omega  -11.00   83.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       15.6827   77.0000 -150.0000 94

  3 omega  -44.00   50.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0890   77.0000  -60.0000 94

  4 omega  -52.00  -25.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       15.6827  -77.0000  120.0000 27
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_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_12      -0.0620481000
_diffrn_orient_matrix_UB_13      0.0136966000
_diffrn_orient_matrix_UB_21      0.0064284000
_diffrn_orient_matrix_UB_22      -0.0269137000
_diffrn_orient_matrix_UB_23      -0.0314532000
_diffrn_orient_matrix_UB_31      0.1185988000
_diffrn_orient_matrix_UB_32      0.0026446000
_diffrn_orient_matrix_UB_33      0.0019085000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7670
_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         25.649
_diffrn_reflns_theta_min         3.536
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.6050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1682
_reflns_number_total             2454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03601g2.cif
_cod_data_source_block           141222-1z
_cod_depositor_comments
'Adding full bibliography for 7709271--7709278.cif.'
_cod_database_code               7709271
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.906
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_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              78278
_shelx_hkl_checksum              19827
_olex2_submission_special_instructions 'No special instructions were received'