A dipotassium 1,2,4-diazaphospholide dianion radical as an organometallic building block: the first 1,2-diaza-4-phosphine ruthenocene.
Zhang, Xiang; Guo, Qiang; Zhang, Yuchen; Zhang, Yaona; Zheng, Wenjun; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13332–13336; doi:10.1039/c8dt03185a

data_7047378
_publ_section_title
;
 A dipotassium 1,2,4-diazaphospholide dianion radical as an organometallic
 building block: the first 1,2-diaza-4-phosphine ruthenocene.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13332
_journal_page_last               13336
_journal_paper_doi               10.1039/c8dt03185a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C48 H50 N4 P2 Ru2, C4 H8 O'
_chemical_formula_sum            'C52 H58 N4 O P2 Ru2'
_chemical_formula_weight         1019.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-25
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2018-06-11 deposited with the CCDC.
2018-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.0606(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3240(2)
_cell_length_b                   15.3663(2)
_cell_length_c                   15.3059(3)
_cell_measurement_reflns_used    18959
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8130
_cell_measurement_theta_min      3.1480
_cell_volume                     2571.87(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
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_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 0.9982
_diffrn_measured_fraction_theta_max 0.9404
_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    -53.00  85.00   1.00    1.50    --   15.84   0.00  90.00  138
  2  \w    -51.00  33.00   1.00    1.50    --   15.84 -57.00 -30.00   84
  3  \w    -14.00  87.00   1.00    1.50    --   15.84  19.00 -90.00  101
  4  \w     -3.00  85.00   1.00    1.50    --   15.84  37.00 150.00   88
  5  \w     -3.00  85.00   1.00    1.50    --   15.84  37.00 -30.00   88
  6  \w     -3.00  85.00   1.00    1.50    --   15.84  37.00  60.00   88
  7  \w    -25.00  22.00   1.00    1.50    --  -17.40 -99.00 150.00   47
  8  \w    -74.00  -1.00   1.00    1.50    --  -17.40 130.00-140.17   73
  9  \w    -70.00   5.00   1.00    1.50    --  -17.40 123.00  32.49   75
 10  \w    -69.00   6.00   1.00    1.50    --  -17.40 121.00 138.49   75
 11  \w    -69.00   6.00   1.00    1.50    --  -17.40 121.00 -13.70   75
 12  \w    -75.00  -1.00   1.00    1.50    --  -17.40 132.00 -80.85   74
 13  \w    -74.00  -1.00   1.00    1.50    --  -17.40 131.00  71.90   73
 14  \w    -25.00  17.00   1.00    1.50    --  -17.40 -99.00-180.00   42
 15  \w    -25.00  22.00   1.00    1.50    --  -17.40 -99.00 -30.00   47
;
_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      0.0608858000
_diffrn_orient_matrix_UB_12      -0.0029901000
_diffrn_orient_matrix_UB_13      -0.0039627000
_diffrn_orient_matrix_UB_21      0.0185440000
_diffrn_orient_matrix_UB_22      0.0319878000
_diffrn_orient_matrix_UB_23      0.0342241000
_diffrn_orient_matrix_UB_31      0.0124181000
_diffrn_orient_matrix_UB_32      -0.0331397000
_diffrn_orient_matrix_UB_33      0.0334286000
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59056
_diffrn_reflns_theta_full        25.65
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51360
_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            orange
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4880
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0802P)^2^+2.8876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                4156
_reflns_number_total             4880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt03185a2.cif
_cod_data_source_block           20161011
_cod_depositor_comments          'Adding full bibliography for 7047378.cif.'
_cod_original_cell_volume        2571.86(8)
_cod_database_code               7047378
_reflns_odcompleteness_completeness 99.82
_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. Restrained distances
 C25-C26 = C26-C27 = C27-C28
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C27 \\sim C28 \\sim O1: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Fixed Sof: C25(0.5) H25A(0.5) H25B(0.5) C26(0.5) H26A(0.5) H26B(0.5) C27(0.5)
 H27A(0.5) H27B(0.5) C28(0.5) H28A(0.5) H28B(0.5) O1(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
5.b 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)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.620
_oxdiff_exptl_absorpt_empirical_full_min 0.777