Shape-persistent, ruthenium(ii)- and iron(ii)-bisterpyridine metallodendrimers: synthesis, traveling-wave ion-mobility mass spectrometry, and photophysical properties
Wang, Jin-Liang; Li, Xiaopeng; Shreiner, Carol D.; Lu, Xiaocun; Moorefield, Charles N.; Tummalapalli, Sreedhar R.; Medvetz, Douglas A.; Panzner, Matthew J.; Fronczek, Frank R.; Wesdemiotis, Chrys; Newkome, George R.; New Journal of Chemistry 36 (2012) 484–; doi:10.1039/c2nj20799k

data_7052824
_publ_section_title
;
 Shape-persistent, ruthenium(ii)- and iron(ii)-bisterpyridine
 metallodendrimers: synthesis, traveling-wave ion-mobility mass
 spectrometry, and photophysical properties
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              484
_journal_paper_doi               10.1039/c2nj20799k
_journal_volume                  36
_journal_year                    2012
_chemical_formula_moiety         'C120 H90 N18 O3 Ru3, 6(N O3), 12(C H4 O)'
_chemical_formula_sum            'C132 H138 N24 O33 Ru3'
_chemical_formula_weight         2891.87
_chemical_name_common            NA
_chemical_name_systematic
;
?
;
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   31.823(7)
_cell_length_b                   31.823(7)
_cell_length_c                   21.495(5)
_cell_measurement_reflns_used    7078
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.38
_cell_measurement_theta_min      2.22
_cell_volume                     18852(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1241
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37,791
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8964
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;Platon squeeze was used to remove a total of 1844 total electons
from three symmetry related voids. Only one of two nitrate anions
was found from the difference map. Removal of the second NO3- results
in 558 e-. As the crystals of compound G0 were
grown from MeOH it is assumed the remaining disordered solvet squeezed
from the model correspond to MeOH solvate molecules. This corresponds to
12 MeOH per molecule of G0 to account for the remaining squeezed e-.
The formula and corresponding values reflect these additions.
;
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.32(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                3126
_reflns_number_total             4121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj20799k.txt
_cod_data_source_block           G0
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        18851(8)
_cod_original_sg_symbol_H-M      R3c
_cod_database_code               7052824