Unsymmetrical PNP-Pincer Type Phosphaalkene Ligands Protected by a Fused-Ring Bulky Eind Group: Synthesis and Applications to Rh(I) and Ir(I) Complexes
Taguchi, Hiro-omi; Sasaki, Daichi; Takeuchi, Katsuhiko; Tsujimoto, Shota; Matsuo, Tsukasa; Tanaka, Hiromasa; Yoshizawa, Kazunari; Ozawa, Fumiyuki; Organometallics 35 (2016) 1526–; doi:10.1021/acs.organomet.6b00113

data_4088464
_publ_section_title
;
 Unsymmetrical PNP-Pincer Type Phosphaalkene Ligands Protected by a
 Fused-Ring Bulky Eind Group: Synthesis and Applications to Rh(I) and
 Ir(I) Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1526
_journal_paper_doi               10.1021/acs.organomet.6b00113
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C65 H102 Cl Ir K N O6 P2'
_chemical_formula_weight         1322.17
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.227(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.222(3)
_cell_length_b                   29.346(8)
_cell_length_c                   18.875(5)
_cell_measurement_reflns_used    13869
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.6060
_cell_measurement_theta_min      1.7189
_cell_volume                     6562(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54836
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7957
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Darkgreen
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.927
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         11540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                9366
_reflns_number_total             11540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00113_si_002.cif
_cod_data_source_block           complex_[K(18c6)][13]
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4088464