The Importance of Kinetic and Thermodynamic Control when Assessing Mechanisms of Carboxylate-Assisted C-H Activation.
Alharis, Raed A.; McMullin, Claire L.; Davies, David L.; Singh, Kuldip; Macgregor, Stuart A.; Journal of the American Chemical Society 141 (2019) 8896–8906; doi:10.1021/jacs.9b02073

data_4127568
_publ_section_title
;
 The Importance of Kinetic and Thermodynamic Control when Assessing
 Mechanisms of Carboxylate-Assisted C-H Activation.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8896
_journal_page_last               8906
_journal_paper_doi               10.1021/jacs.9b02073
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C20 H21 Cl F3 N2 Rh, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C20.5 H22 Cl2 F3 N2 Rh'
_chemical_formula_weight         527.21
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.896(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.863(7)
_cell_length_b                   15.107(7)
_cell_length_c                   19.157(8)
_cell_measurement_reflns_used    649
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.519
_cell_measurement_theta_min      2.182
_cell_volume                     4193(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.2178
_diffrn_reflns_av_sigmaI/netI    0.2363
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32552
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 3857 reflections(SADABS);Rint 0.0972 before
correction and 0.0673 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8239
_refine_ls_number_restraints     559
_refine_ls_restrained_S_all      0.827
_refine_ls_R_factor_all          0.1642
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                3952
_reflns_number_total             8239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b02073_si_003.cif
_cod_data_source_block           3b-CF3_14073
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C41 H44 Cl4 F6 N4 Rh2'
_cod_original_formula_weight         1054.42
_cod_original_formula_moiety         '2(C20 H21 Cl F3 N2 Rh), C H2 Cl2'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4127568