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_7044556
_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 H46 Cl Ir N P2, B F4'
_chemical_formula_sum            'C23 H46 B Cl F4 Ir N P2'
_chemical_formula_weight         713.01
_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
_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                   9.7215(4)
_cell_length_b                   16.4551(7)
_cell_length_c                   18.1397(8)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.351
_cell_measurement_theta_min      2.377
_cell_volume                     2901.8(2)
_computing_cell_refinement
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material
'XCIF program, PLATON(Spek, 1998), PARST(Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker APEX DUO CCD system'
_diffrn_measurement_method       'narrow \w frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24563
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         29.668
_diffrn_reflns_theta_min         1.671
_exptl_absorpt_coefficient_mu    4.842
_exptl_absorpt_correction_T_max  0.5257
_exptl_absorpt_correction_T_min  0.3260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.719
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 3061 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(4)
_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     317
_refine_ls_number_reflns         7497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.885
_reflns_number_gt                7230
_reflns_number_total             7497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03327c2.cif
_cod_data_source_block           cmpnd_2
_cod_database_code               7044556
_shelxl_version_number           2014-3
_shelx_res_checksum              13207