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_4342010
_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         'C27 H22 Mn N4 O5 Rh'
_chemical_formula_sum            'C27 H22 Mn N4 O5 Rh'
_chemical_formula_weight         640.33
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                98.187(2)
_cell_angle_beta                 111.431(2)
_cell_angle_gamma                113.2530(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7295(7)
_cell_length_b                   11.5936(7)
_cell_length_c                   12.5401(13)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.869
_cell_measurement_theta_min      2.202
_cell_volume                     1256.93(18)
_computing_cell_refinement       'CELLNOW, SAINT (Bruker AXS)'
_computing_data_collection       'COSMO (Bruker AXS)'
_computing_data_reduction        'TWINABS (Bruker AXS)'
_computing_molecular_graphics    'Mercury (CCDC)'
_computing_publication_material  'APEX2 (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 0.995
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5848
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.925
_diffrn_reflns_theta_min         1.852
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  0.8399
_exptl_absorpt_correction_T_min  0.7289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
5957 Corrected reflections written to file twin4.hkl
 Reflections merged according to point-group -1    
 Minimum and maximum apparent transmission:  0.681501  0.745622
 Additional spherical absorption correction applied with mu*r =  0.2000

 HKLF 5 dataset constructed from all observations involving domain 2
    8021 Corrected reflections written to file twin5.hkl
 Reflections merged according to point-group -1    
 Single reflections that also occur in composites omitted
 Minimum and maximum apparent transmission:  0.679403  0.745622
 Additional spherical absorption correction applied with mu*r =  0.2000
;
_exptl_crystal_colour            black-green
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0269P)^2^+0.3603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5358
_reflns_number_total             5848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502414r_si_003.cif
_cod_data_source_block           solve_2
_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_original_cell_volume        1256.93(17)
_cod_database_code               4342010
_shelx_estimated_absorpt_t_min   0.729
_shelx_estimated_absorpt_t_max   0.840
_shelxl_version_number           2013-3
_shelx_res_checksum              51864
_shelx_hkl_checksum              38423