Heterobimetallic Complexes of Rhodium Dibenzotetramethylaza[14]annulene [(tmtaa)Rh-M]: Formation, Structures, and Bond Dissociation Energetics.
Imler, Gregory H.; Peters, Garvin M.; Zdilla, Michael J.; Wayland, Bradford B.; Inorganic chemistry 54 (2015) 273–279; doi:10.1021/ic502414r

data_4342011
_publ_section_title
;
 Heterobimetallic Complexes of Rhodium Dibenzotetramethylaza[14]annulene
 [(tmtaa)Rh-M]: Formation, Structures, and Bond Dissociation Energetics.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              273
_journal_page_last               279
_journal_paper_doi               10.1021/ic502414r
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C29 H27 Fe N4 O2 Rh'
_chemical_formula_sum            'C29 H27 Fe N4 O2 Rh'
_chemical_formula_weight         622.30
_chemical_melting_point          ?
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 115.5590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5043(8)
_cell_length_b                   9.4951(4)
_cell_length_c                   17.6056(8)
_cell_measurement_temperature    100(2)
_cell_volume                     2489.0(2)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'SADABS (Bruker-AXS)'
_computing_molecular_graphics    'Mercury (CCDC)'
_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_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_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28834
_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         27.875
_diffrn_reflns_theta_min         1.368
_exptl_absorpt_coefficient_mu    1.281
_exptl_absorpt_correction_T_max  0.9271
_exptl_absorpt_correction_T_min  0.8410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
   30072 Corrected reflections written to file 
 C:\Frames\guest\1294\work\mo_1294_0m.hkl
 Estimated minimum and maximum transmission:  0.6745  0.7456
 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_density_diffrn    1.661
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0291P)^2^+1.3093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4982
_reflns_number_total             5933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502414r_si_004.cif
_cod_data_source_block           mo_1294_0m
_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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4342009--4342012.cif.
;
_cod_database_code               4342011
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.927
_shelxl_version_number           2013-4
_shelx_res_checksum              71384
_shelx_hkl_checksum              84622