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_7127995
_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         'C34 H58 Fe2 P3, C14 H24 N4 P'
_chemical_formula_sum            'C48 H82 Fe2 N4 P4'
_chemical_formula_weight         950.75
_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
_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                90
_cell_angle_beta                 99.5490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7995(2)
_cell_length_b                   22.0551(3)
_cell_length_c                   16.5807(2)
_cell_measurement_reflns_used    11563
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.0320
_cell_measurement_theta_min      3.3740
_cell_volume                     4976.40(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_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 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_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    -19.00  25.00   0.50    1.00    --  -44.92  37.00  90.00   88
  2  \w      2.00  29.00   0.50    1.00    --  -44.92  19.00-150.00   54
  3  \w     -1.00  28.00   0.50    1.00    --  -44.92  19.00-120.00   58
  4  \w     -5.00  31.00   0.50    1.00    --  -44.92  19.00 120.00   72
  5  \w     30.00  96.00   0.50    1.00    --   44.92-125.00 -30.00  132
  6  \w     40.00  93.00   0.50    5.00    --  104.50 -61.00 -60.00  106
  7  \w     23.00 106.00   0.50    5.00    --  104.50 -94.00-180.00  166
  8  \w     33.00  63.00   0.50    5.00    --  104.50-125.00  90.00   60
  9  \w     68.00 178.00   0.50    5.00    --  104.50  15.00 150.00  220
 10  \w     72.00 112.00   0.50    5.00    --  104.50-125.00  90.00   80
 11  \w     36.00  62.00   0.50    5.00    --  104.50 -45.00  30.00   52
 12  \w     45.00  70.00   0.50    5.00    --  104.50 -45.00 -60.00   50
 13  \w     35.00  90.00   0.50    5.00    --  104.50 -61.00-150.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20961
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.005
_diffrn_reflns_theta_min         3.365
_exptl_absorpt_coefficient_mu    6.156
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.044
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.48a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark pink'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.713
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9772
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0852P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9039
_reflns_number_total             9772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00615k2.cif
_cod_data_source_block           abs_det_gaus
_cod_depositor_comments
'Adding full bibliography for 7127994--7127996.cif.'
_cod_database_code               7127995
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.182
_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. Restrained distances
 C14-C16A \\sim C14-C16B
 with sigma of 0.02
 C14-C17A \\sim C14-C17B
 with sigma of 0.02
 C14-C15A \\sim C14-C15B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16B \\sim C16A \\sim C17B \\sim C14 \\sim C17A \\sim C15B \\sim C15A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
4. Others
 Fixed Sof: C16A(0.77) H16A(0.77) H16B(0.77) H16C(0.77) C17A(0.77) H17A(0.77)
 H17B(0.77) H17C(0.77) C15A(0.77) H15A(0.77) H15B(0.77) H15C(0.77) C17B(0.23)
 H17D(0.23) H17E(0.23) H17F(0.23) C15B(0.23) H15D(0.23) H15E(0.23) H15F(0.23)
 C16B(0.23) H16D(0.23) H16E(0.23) H16F(0.23)
5.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C3(H3), C5(H5), C22(H22)
5.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,H34B,
 H34C), C45(H45A,H45B,H45C), C7(H7A,H7B,H7C), C25(H25A,H25B,H25C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C41(H41A,H41B,H41C),
 C48(H48A,H48B,H48C), C33(H33A,H33B,H33C), C24(H24A,H24B,H24C), C39(H39A,H39B,
 H39C), C38(H38A,H38B,H38C), C11(H11A,H11B,H11C), C40(H40A,H40B,H40C), C28(H28A,
 H28B,H28C), C47(H47A,H47B,H47C), C32(H32A,H32B,H32C), C9(H9A,H9B,H9C),
 C46(H46A,H46B,H46C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C15A(H15A,
 H15B,H15C), C17B(H17D,H17E,H17F), C15B(H15D,H15E,H15F), C16B(H16D,H16E,H16F)
;
_shelx_res_checksum              6997
_shelx_hkl_checksum              99194
_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
;