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_4512621
_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         'C4 H12 N2 2+, 2(Br -), H2 O'
_chemical_formula_sum            'C4 H14 Br2 N2 O'
_chemical_formula_weight         265.97
_chemical_name_systematic
; 
 Piperazine-1,4-diium dibromide monohydrate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 108.393(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4831(5)
_cell_length_b                   5.9049(2)
_cell_length_c                   13.9367(6)
_cell_measurement_reflns_used    4576
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      34.26
_cell_measurement_theta_min      3.07
_cell_volume                     896.72(7)
_computing_cell_refinement
; 
CrysAlis Pro ver. 1.171.34.44 (Oxford Diffraction, 2010) 
;
_computing_data_collection
; 
CrysAlis Pro ver. 1.171.34.44 (Oxford Diffraction, 2010) 
;
_computing_data_reduction
; 
CrysAlis Pro ver. 1.171.34.44 (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 16.2711
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos'
_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  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8295
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    8.978
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.22
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlis Pro ver. 1.171.34.44 (Oxford Diffraction, 2010) 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0432(12)
_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   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         927
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0201
_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\^)+(0.0218P)\^2\^+0.5767P] where
 P=(Fo\^2\^+2Fc\^2\^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                823
_reflns_number_total             927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501694d_si_003.cif
_cod_data_source_block           PipBr
_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 'Monoclinic' changed to 'monoclinic'
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.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4512621