Structural and solution equilibrium studies on half-sandwich organorhodium complexes of (N,N) donor bidentate ligands
Mészáros, János P.; Dömötör, Orsolya; Hackl, Carmen M.; Roller, Alexander; Keppler, Bernhard K.; Kandioller, Wolfgang; Enyedy, Éva A.; New Journal of Chemistry 42 (2018) 11174–; doi:10.1039/C8NJ01681J

data_7057473
_publ_section_title
;
 Structural and solution equilibrium studies on half-sandwich
 organorhodium complexes of (N,N) donor bidentate ligands
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11174
_journal_paper_doi               10.1039/C8NJ01681J
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         '3(C16 H31 Cl N2 Rh), 3(C F3 O3 S), 2(H2 O)'
_chemical_formula_sum            'C51 H97 Cl3 F9 N6 O11 Rh3 S3'
_chemical_formula_weight         1652.60
_chemical_name_common            '[Rh(n5-C5Me5)(tmeda)Cl](CF3SO3)'
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-11 deposited with the CCDC.
2018-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5748(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0112(4)
_cell_length_b                   37.6730(11)
_cell_length_c                   13.6054(4)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.374
_cell_measurement_theta_min      2.196
_cell_volume                     6666.5(3)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_collection       APEX2
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41099
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.592
_diffrn_source                   'sealed xray tube'
_diffrn_source_type              'INCOATEC microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0572 before and 0.0364 after correction. 
The Ratio of minimum to maximum transmission is 0.9164. 
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.242
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         12198
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0216P)^2^+7.5091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10138
_reflns_number_total             12198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj01681j2.cif
_cod_data_source_block           caha428_p21n
_cod_depositor_comments
'Adding full bibliography for 7057472--7057474.cif.'
_cod_database_code               7057473
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.711