Half-Sandwich Complexes of Ir(III), Rh(III) and Ru(II) with the MaxPhos Ligand: Metal Centred Chirality and Cyclometallation
Téllez, Juan; Gallen, Albert; Ferrer, Joaquina; Lahoz, Fernando J.; García-Orduña, Pilar; Riera, Antoni; Verdaguer, Xavier; Carmona, Daniel; Grabulosa, Arnald; Dalton Trans.  (2017) –; doi:10.1039/C7DT03327C

data_7044555
_publ_section_title
;
 Half-Sandwich Complexes of Ir(III), Rh(III) and Ru(II) with the MaxPhos
 Ligand: Metal Centred Chirality and Cyclometallation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03327C
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C23 H45 Cl N P2 Ru, F6 P'
_chemical_formula_sum            'C23 H45 Cl F6 N P3 Ru'
_chemical_formula_weight         679.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-06 deposited with the CCDC.
2017-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8826(6)
_cell_length_b                   16.1242(8)
_cell_length_c                   17.1538(8)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.44
_cell_measurement_theta_min      3.28
_cell_volume                     3010.0(3)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31150
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         39.452
_diffrn_reflns_theta_min         3.024
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '0.3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       Block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 5468 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         14925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.2861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0518
_reflns_Friedel_coverage         0.633
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.703
_reflns_number_gt                14345
_reflns_number_total             14925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03327c2.cif
_cod_data_source_block           cmpnd_3prime
_cod_database_code               7044555
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.735
_shelx_estimated_absorpt_t_max   0.853
_shelxl_version_number           2014-3
_shelx_res_checksum              47877