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_7709278
_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         '2(C72 H72 N8 Na4 O4 P4), 8(C7 H8)'
_chemical_formula_sum            'C200 H208 N16 Na8 O8 P8'
_chemical_formula_weight         3395.50
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-01-23
_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            2
_cell_length_a                   27.3350(10)
_cell_length_b                   27.3350(10)
_cell_length_c                   12.7837(9)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0910
_cell_measurement_theta_min      3.3980
_cell_volume                     9552.0(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0251
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9371
_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     -1.00  83.00   1.00  125.11    --   15.84  57.00 150.00   84
  2  \w    -51.00  33.00   1.00  125.11    --   15.84 -57.00   0.00   84
  3  \w    -51.00  33.00   1.00  125.11    --   15.84 -57.00-120.00   84
  4  \w     -3.00  85.00   1.00  125.11    --   15.84  37.00  30.00   88
  5  \w    -11.00  83.00   1.00  125.11    --   15.84  77.00-120.00   94
  6  \w    -25.00  22.00   1.00  125.11    --  -17.40 -99.00  30.00   47
  7  \w    -25.00  30.00   1.00  125.11    --   15.84 -99.00-150.00   55
  8  \w     32.00  88.00   1.00  125.11    --   15.84-178.00-150.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0259441000
_diffrn_orient_matrix_UB_12      0.0005469000
_diffrn_orient_matrix_UB_13      0.0008523000
_diffrn_orient_matrix_UB_21      0.0005840000
_diffrn_orient_matrix_UB_22      0.0259266000
_diffrn_orient_matrix_UB_23      0.0013587000
_diffrn_orient_matrix_UB_31      -0.0005503000
_diffrn_orient_matrix_UB_32      0.0006473000
_diffrn_orient_matrix_UB_33      -0.0554627000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            53479
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4507
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0785
_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^)+(0.1475P)^2^+10.9446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2344
_refine_ls_wR_factor_ref         0.2576
_reflns_number_gt                3331
_reflns_number_total             4507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt03601g2.cif
_cod_data_source_block           20201229-1
_cod_depositor_comments
'Adding full bibliography for 7709271--7709278.cif.'
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7709278
_reflns_odcompleteness_completeness 99.80
_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
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B)
3.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
3.d Fitted hexagon refined as free rotating group:
 C19(C20,C21,C22,C23,C24)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.593
_oxdiff_exptl_absorpt_empirical_full_min 0.681