Isolation of Au-, Co-η1PCO and Cu-η2PCO complexes, conversion of an Ir‒η1PCO complex into a dimetalladiphosphene, and an interaction-free PCO anion
Liu, Liu; Ruiz, David A.; Dahcheh, Fatme; Bertrand, Guy; Suter, Riccardo; Tondreau, Aaron M.; Grützmacher, Hansjörg; Chem. Sci. 7 (2016) 2335–; doi:10.1039/C5SC04504E

data_1541893
_publ_section_title
;
 Isolation of Au-, Co-\h1PCO and Cu-\h2PCO complexes, conversion of an
 Ir--\h1PCO complex into a dimetalladiphosphene, and an interaction-free
 PCO anion
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2335
_journal_paper_doi               10.1039/C5SC04504E
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C34 H43 Co N3 O P, 2(C4 H8 O)'
_chemical_formula_sum            'C42 H59 Co N3 O3 P'
_chemical_formula_weight         743.82
_chemical_name_systematic        iPr(PDI)Co(PCO)
_chemical_properties_physical    'Air-sensitive, Heat-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-12 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                111.476(4)
_cell_angle_beta                 93.948(4)
_cell_angle_gamma                104.766(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1044(5)
_cell_length_b                   14.1614(7)
_cell_length_c                   15.8020(7)
_cell_measurement_reflns_used    7587
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      28.8370
_cell_measurement_theta_min      3.1910
_cell_volume                     2001.36(19)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(2)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -11.00   14.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000  -90.0000 25

  2 omega  -21.00   20.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   60.0000 41

  3 omega  -98.00  -34.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904 -179.0000  -90.0000 64

  4 omega    1.00   28.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   38.0000   90.0000 27

  5 omega   21.00   67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000 -120.0000 46

  6 omega   41.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   38.0000   90.0000 53

  7 omega  -24.00    7.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -57.0000  150.0000 31

  8 omega  -44.00   -4.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -77.0000  150.0000 40

  9 omega   13.00   52.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -77.0000  150.0000 39

 10 omega    6.00   88.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000  -60.0000 82

 11 omega  -52.00    5.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   77.0000  -90.0000 57

 12 omega  -47.00   44.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -57.0000   60.0000 91

 13 omega    1.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000   30.0000 90

 14 omega   34.00   98.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  179.0000    0.0000 64

 15 omega    1.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000 -180.0000 90
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_UB_11      -0.0329899000
_diffrn_orient_matrix_UB_12      -0.0357930000
_diffrn_orient_matrix_UB_13      0.0193599000
_diffrn_orient_matrix_UB_21      -0.0615107000
_diffrn_orient_matrix_UB_22      -0.0169284000
_diffrn_orient_matrix_UB_23      -0.0329665000
_diffrn_orient_matrix_UB_31      0.0239754000
_diffrn_orient_matrix_UB_32      -0.0402437000
_diffrn_orient_matrix_UB_33      -0.0307127000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30723
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_preparation       'Na(OCP) and (iPrPDI)CoCl in thf'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf hexanes'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8175
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0712
_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^)+(0.0380P)^2^+1.8930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7094
_reflns_number_total             8175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04504e2.cif
_cod_data_source_block           mepdiirpco2
_cod_depositor_comments
'Adding full bibliography for 1541885--1541894.cif.'
_cod_original_cell_volume        2001.36(18)
_cod_database_code               1541893
_chemical_oxdiff_formula         Co1P1C50H50N2
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 C44-C43 = C42-C41 = C41-C40 = C40-C39 = C46-C45 = C46-C43
 1.48721 with sigma of 0.001
 O3-C42 = O3-C39 = O4-C44 = O4-C45
 1.48721 with sigma of 0.001
3. Rigid body (RIGU) restrains
 C44, C43, C46, C45, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(O4)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(O3)=FVAR(1)
 1(DFIX)=1(DFIX)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C16(H16), C31(H31), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C14(H14), C13(H13), C12(H12), C26(H26), C25(H25),
 C24(H24)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              57416
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'