Equilibrium Thermodynamics To Form a Rhodium Formyl Complex from Reactions of CO and H2: Metal σ Donor Activation of CO.
Imler, Gregory H.; Zdilla, Michael J.; Wayland, Bradford B.; Journal of the American Chemical Society 136 (2014) 5856–5859; doi:10.1021/ja501173d

data_4121676
_publ_section_title
;
 Equilibrium Thermodynamics To Form a Rhodium Formyl Complex from
 Reactions of CO and H2: Metal \s Donor Activation of CO.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5856
_journal_page_last               5859
_journal_paper_doi               10.1021/ja501173d
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C23 H23 N4 O Rh'
_chemical_formula_sum            'C23 H23 N4 O Rh'
_chemical_formula_weight         474.36
_chemical_melting_point          ?
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                81.340(4)
_cell_angle_beta                 82.196(4)
_cell_angle_gamma                77.787(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4476(13)
_cell_length_b                   10.5579(16)
_cell_length_c                   12.962(2)
_cell_measurement_reflns_used    3650
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3645
_cell_measurement_theta_min      2.705
_cell_volume                     1110.5(3)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'SADABS (Bruker-AXS)'
_computing_molecular_graphics    XP
_computing_publication_material  'APEX2 report generator (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Kappa APEX II DUO'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         1.598
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.9691
_exptl_absorpt_correction_T_min  0.9113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  17647 Corrected reflections written to file mo_1165_0m.hkl
 Estimated minimum and maximum transmission:  0.6956  0.7464
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2000
 Lambda/2 correction factor = 0.0015
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
One disorderd toluene molecule was removed using SQUEEZE. The number
of electrons calculated by SQUEEZE was 33 compared to the 
theoretical 50 for a toluene molecule. 
;
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4275
_reflns_number_total             5288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja501173d_si_002.cif
_cod_data_source_block           squeeze-sr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not determined' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4121676--4121677.cif.
;
_cod_database_code               4121676
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2013-4
_shelx_res_checksum              49611
_shelx_hkl_checksum              48195