Gas-phase reactivity of Cp* Group IX metal complexes bearing aromatic N,N’-chelating ligands
Kerner, Christian; Neu, Jens P.; Gaffga, Maximilian; Lang, Johannes; Oelkers, Benjamin; Sun, Yu; Niedner-Schatterburg, Gereon; Thiel, Werner R.; New J. Chem. 41 (2017) 6995–7006; doi:10.1039/C7NJ01079F

data_7056175
_publ_section_title
;
 Gas-phase reactivity of Cp* Group IX metal complexes bearing aromatic
 N,N&#x2019;-chelating ligands
;
_journal_issue                   15
_journal_name_full               'New J. Chem.'
_journal_page_first              6995
_journal_page_last               7006
_journal_paper_doi               10.1039/C7NJ01079F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C20 H23 Cl F6 N2 P Rh'
_chemical_formula_weight         574.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-31 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9323(3)
_cell_length_b                   8.1971(2)
_cell_length_c                   10.4445(3)
_cell_measurement_reflns_used    4569
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.6260
_cell_measurement_theta_min      5.3920
_cell_volume                     1107.19(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Giacovazzo et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1399
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6409
_diffrn_reflns_point_group_measured_fraction_full 0.813
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        62.686
_diffrn_reflns_theta_max         62.686
_diffrn_reflns_theta_min         5.397
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.592
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.213
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 509 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(12)
_refine_ls_extinction_coef       0.0037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1515
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0487P)^2^+0.0459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.533
_reflns_Friedel_fraction_full    0.603
_reflns_Friedel_fraction_max     0.602
_reflns_number_gt                1498
_reflns_number_total             1515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01079f2.cif
_cod_data_source_block           shelx
_cod_database_code               7056175
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.139
_shelx_estimated_absorpt_t_max   0.262
_shelx_res_checksum              40613