Efficient Diffusion-Controlled Ligand Exchange Crystal Growth of Isostructural Inorganic‒Organic Halogenidorhodates(III): The Missing Hexaiodidorhodate(III) Anion
Bujak, Maciej; Crystal Growth & Design 15 (2015) 1295–; doi:10.1021/cg501694d

data_4512619
_publ_section_title
;
 Efficient Diffusion-Controlled Ligand Exchange Crystal Growth of
 Isostructural Inorganic--Organic Halogenidorhodates(III): The Missing
 Hexaiodidorhodate(III) Anion
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1295
_journal_paper_doi               10.1021/cg501694d
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         '2(C4 H12 N2 2+), Rh Br6 3-, Br -, H2 O'
_chemical_formula_sum            'C8 H26 Br7 N4 O Rh'
_chemical_formula_weight         856.54
_chemical_name_systematic
; 
Piperazine-1,4-diium hexabromidorhodate(III) bromide monohydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.3712(9)
_cell_length_b                   10.1433(5)
_cell_length_c                   7.9013(3)
_cell_measurement_reflns_used    7913
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      31.17
_cell_measurement_theta_min      1.54
_cell_volume                     2113.53(15)
_computing_cell_refinement
; 
  CrysAlis Pro ver. 1.171.33.61 (Oxford Diffraction, 2010) 
;
_computing_data_collection
; 
 KUMA Diffraction Instruments, UNIL IC and KUMA Diffration Data 
 collection GUI for CCD, version 1.166 (KUMA, 2000) 
;
_computing_data_reduction
; 
  CrysAlis Pro ver. 1.171.33.61 (Oxford Diffraction, 2010)
;
_computing_molecular_graphics    'Mercury (Macrae at al., 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.3167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STADI4 CCD'
_diffrn_measurement_method       \w-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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            22021
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    14.045
_exptl_absorpt_correction_T_max  0.26
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlis Pro ver. 1.171.33.61 (Oxford Diffraction, 2010)  
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00217(5)
_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_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2091
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0343
_refine_ls_wR_factor_ref         0.0359
_reflns_number_gt                1510
_reflns_number_total             2091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501694d_si_003.cif
_cod_data_source_block           PipRhBr
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4512619--4512622.cif.
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_cod_database_code               4512619