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_7057472
_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_absolute_configuration ad
_chemical_formula_moiety         'C14 H27 Cl N2 Rh, C F3 O3 S'
_chemical_formula_sum            'C15 H27 Cl F3 N2 O3 Rh S'
_chemical_formula_weight         510.80
_chemical_name_common            '[Rh (n5-C5Me5)(dmen)Cl](CF3SO3)'
_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   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5159(3)
_cell_length_b                   9.7262(4)
_cell_length_c                   24.5900(10)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.136
_cell_measurement_theta_min      2.530
_cell_volume                     2036.72(14)
_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 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            77632
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.131
_diffrn_reflns_theta_min         2.252
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0750 before and 0.0369 after correction. 
The Ratio of minimum to maximum transmission is 0.9374. 
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    1.666
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.266
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2558 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.024(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0138
_refine_ls_R_factor_gt           0.0135
_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^)+(0.0168P)^2^+0.5591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0342
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5929
_reflns_number_total             5994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj01681j2.cif
_cod_data_source_block           caha427_p212121
_cod_depositor_comments
'Adding full bibliography for 7057472--7057474.cif.'
_cod_database_code               7057472
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.677