1,2-Diaza-4-phosphaferrocenes: Synthesis, Structural Characterization, 57Fe Mössbauer Spectrum Analysis, and DFT Calculation
Zheng, Wenjun; Duan, Lian; Zhang, Xiang; Dalton Trans.  (2017) –; doi:10.1039/C7DT01732D

data_7043278
_publ_section_title
;
 1,2-Diaza-4-phosphaferrocenes: Synthesis, Structural Characterization,
 57Fe M\"ossbauer Spectrum Analysis, and DFT Calculation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01732D
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H25 Fe N2 P'
_chemical_formula_sum            'C24 H25 Fe N2 P'
_chemical_formula_weight         428.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_primary     direct
_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
;
2017-06-02 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.917(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7621(4)
_cell_length_b                   7.4818(2)
_cell_length_c                   17.8088(4)
_cell_measurement_reflns_used    2104
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      70.3420
_cell_measurement_theta_min      6.5680
_cell_volume                     2088.98(9)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9946
_diffrn_measured_fraction_theta_max 0.5780
_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     33.00 122.00   1.00    1.07    --   54.00  57.00 -90.00   89
  2  \w     88.00 121.00   1.00    1.07    --   54.00  57.00 -60.00   33
  3  \w    142.00 177.00   1.00    1.07    --  108.00  37.00   0.00   35
  4  \w    102.00 156.00   1.00    1.07    --  108.00 111.00  90.00   54
  5  \w     95.00 168.00   1.00    1.07    --  108.00  63.00 150.00   73
  6  \w     40.00  70.00   1.00    1.07    --   54.00  57.00 150.00   30
  7  \w     38.00 118.00   1.00    1.07    --  108.00 -50.00  30.00   80
  8  \w     44.00 102.00   1.00    1.07    --  108.00-111.00 -30.00   58
  9  \w     42.00 116.00   1.00    1.07    --  108.00-111.00  60.00   74
 10  \w     32.00 107.00   1.00    1.07    --   54.00-125.00 -30.00   75
 11  \w     11.00  59.00   1.00    1.07    --   54.00 -57.00 150.00   48
 12  \w    -24.00  18.00   1.00    1.00    --    0.00 -37.00 120.00   42
 13  \w    -69.00 -39.00   1.00    1.00    --    0.00 -37.00 120.00   30
 14  \w     93.00 119.00   1.00    1.07    --  108.00  63.00-180.00   26
 15  \w    139.00 176.00   1.00    1.07    --  108.00  63.00-180.00   37
 16  \w    144.00 169.00   1.00    1.07    --  108.00 111.00-150.00   25
 17  \w    113.00 145.00   1.00    1.07    --  108.00 178.00-120.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0768170000
_diffrn_orient_matrix_UB_12      0.1277360000
_diffrn_orient_matrix_UB_13      0.0015453000
_diffrn_orient_matrix_UB_21      -0.0604781000
_diffrn_orient_matrix_UB_22      0.1611345000
_diffrn_orient_matrix_UB_23      0.0027760000
_diffrn_orient_matrix_UB_31      0.0106354000
_diffrn_orient_matrix_UB_32      -0.0074887000
_diffrn_orient_matrix_UB_33      0.0868943000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3700
_diffrn_reflns_theta_full        67.0539
_diffrn_reflns_theta_max         67.05
_diffrn_reflns_theta_min         6.56
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40993
_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            'clear light yellow'
_exptl_crystal_density_diffrn    1.3617
_exptl_crystal_description       block
_exptl_crystal_F_000             894.6749
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.8825
_refine_diff_density_min         -0.8583
_refine_diff_density_rms         0.1142
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.008(8)
_refine_ls_d_res_high            0.8372
_refine_ls_d_res_low             6.7523
_refine_ls_goodness_of_fit_ref   1.0765
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     257
_refine_ls_number_reflns         2238
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.0637
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.1000
_refine_ls_shift/su_mean         0.0055
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1548P)^2^+1.8072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1862
_reflns_Friedel_coverage         0.205
_reflns_limit_h_max              18
_reflns_limit_h_min              -17
_reflns_limit_k_max              8
_reflns_limit_k_min              -8
_reflns_limit_l_max              21
_reflns_limit_l_min              -14
_reflns_number_gt                2144
_reflns_number_total             2238
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt01732d2.cif
_cod_data_source_block           exp_1677
_cod_database_code               7043278
_chemical_oxdiff_formula         'C1 H1 O1 N1 P1 Zn1'
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(Fe1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a 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)
3.b 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)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.760
_oxdiff_exptl_absorpt_empirical_full_min 0.530