Structural Chemistry of "Defect" Cyanometalate Boxes: {Cs@[CpCo(CN)3]4[Cp*Ru]3} and {M@[Cp*Rh(CN)3]4[Cp*Ru]3} (M = NH4, Cs)
Matthew L. Kuhlman; Thomas B. Rauchfuss; Journal of the American Chemical Society 125 (2003) 10084–10092; doi:10.1021/ja035253h

data_4114070
_publ_section_title
;
 Structural Chemistry of "Defect" Cyanometalate Boxes:
 {Cs@[CpCo(CN)3]4[Cp*Ru]3} and {M@[Cp*Rh(CN)3]4[Cp*Ru]3} (M = NH4, Cs)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10084
_journal_page_last               10092
_journal_paper_doi               10.1021/ja035253h
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C82 H105 Cs N12 Rh4 Ru3, (C2 H3 N)10'
_chemical_formula_sum            'C102 H135 Cs N22 Rh4 Ru3'
_chemical_formula_weight         2517.08
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_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
_audit_update_record
; 
2002-03-11   text and data added, mlk 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.076(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9260(12)
_cell_length_b                   48.475(4)
_cell_length_c                   16.0926(12)
_cell_measurement_reflns_used    1001
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.92
_cell_volume                     11294.0(16)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  p93qas
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            67845
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_time  293
_diffrn_standards_number         1294
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_T_max  0.6957
_exptl_absorpt_correction_T_min  0.4688
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       prism
_exptl_crystal_F_000             5072
_exptl_crystal_id                p93qas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.5 mm 
cryo-loop (Hampton Research) with the (0 -1 0) scattering planes roughly 
normal to the spindle axis. 
;
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         3.225
_refine_diff_density_min         -2.090
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         19946
_refine_ls_number_restraints     994
_refine_ls_restrained_S_all      1.315
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.1215
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+401.6955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2541
_refine_ls_wR_factor_ref         0.2569
_reflns_number_gt                18247
_reflns_number_total             19946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035253hsi20030320_021557.cif
_cod_data_source_block           p93qas
_cod_original_cell_volume        11293.9(15)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4114070