Reactivity of P<sub>4</sub> butterfly complexes towards NHCs - generation of a metal-bridged P<sub>2</sub> dumbbell complex.
Reichl, Stephan; Grünbauer, Rebecca; Balázs, Gábor; Scheer, Manfred; Chemical communications (Cambridge, England) 57 (2021) 3383–3386; doi:10.1039/d1cc00615k

data_7127994
_publ_section_title
;
 Reactivity of P<sub>4</sub> butterfly complexes towards NHCs - generation
 of a metal-bridged P<sub>2</sub> dumbbell complex.
;
_journal_issue                   27
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3383
_journal_page_last               3386
_journal_paper_doi               10.1039/d1cc00615k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C19 H29 Fe O2, C14 H24 N4 P'
_chemical_formula_sum            'C33 H53 Fe N4 O2 P'
_chemical_formula_weight         624.61
_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
_audit_creation_date             2020-04-08
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.04.02 svn.r1fbe7b6f for OlexSys, GUI svn.r6076)
;
_audit_update_record
;
2021-02-02 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                106.563(4)
_cell_angle_beta                 98.875(3)
_cell_angle_gamma                113.707(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8194(4)
_cell_length_b                   12.5965(6)
_cell_length_c                   15.1388(6)
_cell_measurement_reflns_used    7035
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      72.5550
_cell_measurement_theta_min      4.1290
_cell_volume                     1723.64(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.966
_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    -95.00 -18.00   1.00   10.00    --  -40.72 125.00  30.00   77
  2  \w     10.00 117.00   1.00   10.00    --   40.72  77.00-120.00  107
  3  \w      9.00  79.00   1.00   10.00    --   40.72-125.00-180.00   70
  4  \w     23.00 113.00   1.00   10.00    --   40.72  38.00   0.00   90
  5  \w     83.00 112.00   1.00   10.00    --   40.72  38.00  30.00   29
  6  \w     36.00  98.00   1.00   40.00    --  106.97 -91.00 116.12   62
  7  \w     34.00  64.00   1.00   40.00    --  106.97 -30.00-150.00   30
  8  \w     31.00  66.00   1.00   40.00    --  106.97 -30.00 -90.00   35
  9  \w     23.00 147.00   1.00   40.00    --  106.97 -89.00-119.41  124
 10  \w     20.00  60.00   1.00   40.00    --  106.97 -91.00  84.25   40
 11  \w    110.00 169.00   1.00   40.00    --  106.97  45.00-120.00   59
 12  \w     86.00 137.00   1.00   40.00    --  106.97 -91.00 -29.17   51
 13  \w     27.00  81.00   1.00   40.00    --  106.97-111.00  60.00   54
 14  \w     32.00  66.00   1.00   40.00    --  106.97 -30.00 -60.00   34
 15  \w     33.00  71.00   1.00   40.00    --  106.97 -45.00 150.00   38
 16  \w     38.00  65.00   1.00   40.00    --  106.97 -91.00 -29.17   27
 17  \w     24.00 104.00   1.00   40.00    --  106.97 -87.00 164.80   80
 18  \w    119.00 144.00   1.00   40.00    --  106.97 -87.00 164.80   25
 19  \w     29.00  64.00   1.00   40.00    --  106.97 -30.00-120.00   35
 20  \w     74.00 101.00   1.00   40.00    --  106.97 -91.00  84.25   27
 21  \w     31.00 177.00   1.00   40.00    --  106.97  15.00-150.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12167
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.873
_diffrn_reflns_theta_min         4.151
_exptl_absorpt_coefficient_mu    4.198
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.7278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6295
_reflns_number_total             6639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00615k2.cif
_cod_data_source_block           abs_ana_det
_cod_depositor_comments
'Adding full bibliography for 7127994--7127996.cif.'
_cod_original_cell_volume        1723.64(14)
_cod_database_code               7127994
_shelx_shelxl_version_number     2018/3
_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.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C26(H26A,H26B,
 H26C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C10(H10A,H10B,H10C), C30(H30A,
 H30B,H30C), C25(H25A,H25B,H25C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C15(H15A,H15B,H15C), C24(H24A,H24B,
 H24C), C13(H13A,H13B,H13C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              70173
_shelx_hkl_checksum              30385
_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
- Detector area scaling
;