Ester-substituted cyclometallated rhodium and iridium coordination assemblies with π-bonded dioxolene ligand: synthesis, structures and luminescent properties
Damas, Aurelie; Sesolis, Hugo; Rager, Marie Noelle; Chamoreau, Lise Marie; Gullo, Maria Pia; Barbieri, Andrea; Amouri, Hani; RSC Adv. 4 (2014) 23740–; doi:10.1039/C4RA01185F

data_7235529
_publ_section_title
;
 Ester-substituted cyclometallated rhodium and iridium coordination
 assemblies with \p-bonded dioxolene ligand: synthesis, structures and
 luminescent properties
;
_journal_issue                   45
_journal_name_full               'RSC Adv.'
_journal_page_first              23740
_journal_paper_doi               10.1039/C4RA01185F
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C42 H39 Ir N2 O6 Ru, 3(H2 O)'
_chemical_formula_sum            'C42 H45 Ir N2 O9 Ru'
_chemical_formula_weight         1015.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 122.944(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2991(14)
_cell_length_b                   24.5147(15)
_cell_length_c                   18.4529(12)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.27
_cell_volume                     8465.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44781
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.119
_exptl_absorpt_coefficient_mu    3.552
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   0.745
_exptl_transmission_factor_min   0.59
_refine_diff_density_max         2.387
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+128.0674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5257
_reflns_number_total             7451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra01185f2.cif
_cod_data_source_block           ad207_0m
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7235529
_shelxl_version_number           2013-4
_shelx_res_checksum              72122