Alkylammonium Hexachlorometalates. 5.1 Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H~3~N-(CH~2~)~6~-NH~3~]~2~[H~9~O~4~][RhCl~6~]Cl~2~: Chain-like [H~9~O~4~]^+^ Ions Enclosed in the Cavities of a Complex Organic-Inorganic Framework
Walter Frank; Guido J. Reiss; Inorganic Chemistry 36 (1997) 4593–4595; doi:10.1021/ic970337a

data_4323611
_publ_contact_author
;
      Walter Frank
      Fachbereich Chemie
      Universit\"at Kaiserslautern
      Erwin-Schr\"odinger-Stra\&se
      67663 Kaiserslautern
      Bundesrepublik Deutschland
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_publ_contact_author_email       wfrank@chemie.uni-kl.de
_publ_contact_author_fax         '049 631 2053200'
_publ_contact_author_phone       '049 631 2052986'
_publ_section_title
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 Alkylammonium Hexachlorometalates. 5.1 Bis(1,6-diammoniohexane)
 Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride,
 [H~3~N-(CH~2~)~6~-NH~3~]~2~[H~9~O~4~][RhCl~6~]Cl~2~: Chain-like
 [H~9~O~4~]^+^ Ions Enclosed in the Cavities of a Complex
 Organic-Inorganic Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4593
_journal_page_last               4595
_journal_paper_doi               10.1021/ic970337a
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C12 H45 Cl8 N4 O4 Rh'
_chemical_formula_weight         696.03
_chemical_name_systematic
;
Bis(1,6-diammoniohexane) tetraaquahydrogen hexachlororhodate(III) dichloride
;
_chemical_temperature_decomposition 315
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                97.132(5)
_cell_angle_beta                 104.620(7)
_cell_angle_gamma                95.373(6)
_cell_formula_units_Z            1
_cell_length_a                   7.6079(6)
_cell_length_b                   9.1720(5)
_cell_length_c                   10.8972(7)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      11.7
_cell_volume                     723.88(9)
_computing_cell_refinement       'Siemens XSCANS 2.10b'
_computing_data_collection       'Siemens XSCANS 2.10b'
_computing_data_reduction        'Siemens XSCANS 2.10b'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4 4-circle diffractometer'
_diffrn_measurement_method       OMEGA-SCAN
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9171
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       'brick shaped'
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         '1.160 (near Rh)'
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0540(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   2.631
_refine_ls_goodness_of_fit_obs   2.677
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         5178
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      2.621
_refine_ls_restrained_S_obs      2.676
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_obs          0.0277
_refine_ls_shift/esd_max         0.607
_refine_ls_shift/esd_mean        0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0529
_refine_ls_wR_factor_obs         0.0527
_reflns_number_observed          4979
_reflns_number_total             5225
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970337a.cif
_cod_data_source_block
'[H~3~N-(CH~2~)~6~-NH~3~]~2~[H~9~O~4~][RhCl~6~]Cl~2~'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)]' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        723.9(5)
_cod_database_code               4323611