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_7127996
_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         'C26 H39 Cr N4 O2 P2, C13 H15 Cr O3'
_chemical_formula_sum            'C39 H54 Cr2 N4 O5 P2'
_chemical_formula_weight         824.80
_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             2020-02-13
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020)
;
_audit_update_record
;
2021-02-02 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7244(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7956(3)
_cell_length_b                   8.60807(16)
_cell_length_c                   32.9425(6)
_cell_measurement_reflns_used    15253
_cell_measurement_temperature    123.00(16)
_cell_measurement_theta_max      74.4820
_cell_measurement_theta_min      4.6610
_cell_volume                     4157.54(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.970
_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   -130.00 -34.00   1.00    5.00    --  -43.39 178.00  90.00   96
  2  \w    -50.00  28.00   1.00    5.00    --  -43.39  38.00  60.00   78
  3  \w     19.00 115.00   1.00    5.00    --   43.39  38.00 150.00   96
  4  \w     55.00 130.00   1.00    5.00    --   43.39-178.00  30.00   75
  5  \w     75.00 178.00   1.00   25.00    --  107.00  77.00  30.00  103
  6  \w     33.00 117.00   1.00   25.00    --  107.00-125.00 -90.00   84
  7  \w     34.00  90.00   1.00   25.00    --  107.00 -30.00   0.00   56
  8  \w     24.00 109.00   1.00   25.00    --  107.00 -94.00 -60.00   85
  9  \w     80.00 178.00   1.00   25.00    --  107.00  30.00-180.00   98
 10  \w     34.00  90.00   1.00   25.00    --  107.00 -30.00 -90.00   56
 11  \w     24.00 109.00   1.00   25.00    --  107.00 -94.00  30.00   85
 12  \w     83.00 178.00   1.00   25.00    --  107.00  45.00  90.00   95
 13  \w     18.00 113.00   1.00    5.00    --   43.39  57.00 -60.00   95
 14  \w     18.00 113.00   1.00    5.00    --   43.39  57.00-150.00   95
 15  \w     18.00 113.00   1.00    5.00    --   43.39  57.00  30.00   95
 16  \w     83.00 178.00   1.00   25.00    --  107.00  45.00 -30.00   95
 17  \w     34.00  90.00   1.00   25.00    --  107.00 -30.00  60.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0492875000
_diffrn_orient_matrix_UB_12      -0.1577189000
_diffrn_orient_matrix_UB_13      0.0003434000
_diffrn_orient_matrix_UB_21      -0.0765333000
_diffrn_orient_matrix_UB_22      -0.0627172000
_diffrn_orient_matrix_UB_23      -0.0321511000
_diffrn_orient_matrix_UB_31      0.0524362000
_diffrn_orient_matrix_UB_32      0.0569373000
_diffrn_orient_matrix_UB_33      -0.0345392000
_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  0.0616
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            35858
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.267
_diffrn_reflns_theta_min         3.467
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.399
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020)
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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.1663
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.0956
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         8355
_refine_ls_number_restraints     314
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0654P)^2^+1.0555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7041
_reflns_number_total             8355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00615k2.cif
_cod_data_source_block           rg149_mp_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 7127994--7127996.cif.'
_cod_original_cell_volume        4157.52(13)
_cod_database_code               7127996
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C39H54Cr2N4O5P2
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.467
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20A-C19A \\sim C21A-C20A \\sim C21A-C17A \\sim C18A-C17A \\sim C19A-C18A
 with sigma of 0.02
 C19B-C18B \\sim C17B-C18B \\sim C17B-C21B \\sim C21B-C20B \\sim C20B-C19B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C31A \\sim C36A \\sim C32A \\sim C37A \\sim C30A \\sim C35A \\sim C35B \\sim
C30B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 1.7A
C30B \\sim C31A \\sim C31B \\sim C32A \\sim C32B \\sim C33A \\sim C33B \\sim
C34A \\sim C34B \\sim C30A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.02 within 1.7A
C20B \\sim C19A \\sim C19B \\sim C18A \\sim C18B \\sim C17A \\sim C17B \\sim
C21A \\sim C21B \\sim C20A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
4. Others
 Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C30B)=Sof(C31B)=Sof(C36B)=
 Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C32B)=Sof(C37B)=Sof(H37D)=Sof(H37E)=
 Sof(H37F)=Sof(C33B)=Sof(C38B)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C34B)=
 Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(C34A)=Sof(C33A)=Sof(C32A)=Sof(C30A)=Sof(C31A)=Sof(C39A)=Sof(H39A)=
 Sof(H39B)=Sof(H39C)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C35A)=
 Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
 Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C19B)=Sof(C20B)=Sof(C25B)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C21B)=Sof(C26B)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C17B)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C18B)=
 Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(C20A)=Sof(C21A)=Sof(C19A)=Sof(C17A)=Sof(C18A)=Sof(C26A)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C24A)=
 Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
5.a Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C11(H11A,H11B,H11C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C),
 C26A(H26A,H26B,H26C), C22A(H22A,H22B,H22C), C24A(H24A,H24B,H24C), C25A(H25A,
 H25B,H25C), C23A(H23A,H23B,H23C), C39A(H39A,H39B,H39C), C38A(H38A,H38B,H38C),
 C35A(H35A,H35B,H35C), C36A(H36A,H36B,H36C), C37A(H37A,H37B,H37C), C35B(H35D,
 H35E,H35F), C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F), C38B(H38D,H38E,H38F),
 C39B(H39D,H39E,H39F), C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F), C26B(H26D,
 H26E,H26F), C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F)
;
_shelx_res_checksum              56043
_shelx_hkl_checksum              86285
_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 4.329
_oxdiff_exptl_absorpt_empirical_full_min 0.222