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_1541894
_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         'C26 H27 Ir N3 O P'
_chemical_formula_sum            'C30 H35 Ir N3 O2 P'
_chemical_formula_weight         692.8
_chemical_name_common            '[(MePDI)IrCO]2(\m-P2)'
_chemical_name_systematic        '[(MePDI)IrCO]2(\m-P2)'
_chemical_properties_physical    Air-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 96.530(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7808(13)
_cell_length_b                   12.3485(16)
_cell_length_c                   16.5685(19)
_cell_measurement_reflns_used    9257
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.31
_cell_measurement_theta_min      2.46
_cell_volume                     2801.2(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78327
_diffrn_reflns_theta_full        36.39
_diffrn_reflns_theta_max         36.39
_diffrn_reflns_theta_min         2.46
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.855
_exptl_absorpt_correction_T_max  0.5303
_exptl_absorpt_correction_T_min  0.3773
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf / hexanes'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.515
_refine_diff_density_min         -2.308
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         13573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.937
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0471
_reflns_number_gt                10829
_reflns_number_total             13573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04504e2.cif
_cod_data_source_block           mepdiirpco2
_cod_depositor_comments
'Adding full bibliography for 1541885--1541894.cif.'
_cod_original_formula_sum        'C30 H35 Ir1 N3 O2 P1'
_cod_database_code               1541894
_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:
 C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C20(H20), C21(H21),
 C22(H22)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C9(H9a,H9b,H9c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c),
 C24(H24a,H24b,H24c), C25(H25a,H25b,H25c)
;
_olex2_submission_special_instructions 'No special instructions were received'