Novel barium-organic incorporated iodometalates: do they have template properties for constructing rare heterotrimetallic hybrids?
Mishra, Shashank; Jeanneau, Erwann; Ledoux, Gilles; Daniele, Stéphane; Inorganic chemistry 53 (2014) 11721–11731; doi:10.1021/ic501963y

data_4341352
_publ_section_title
;
 Novel barium-organic incorporated iodometalates: do they have template
 properties for constructing rare heterotrimetallic hybrids?
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11721
_journal_page_last               11731
_journal_paper_doi               10.1021/ic501963y
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C22 H48 Ba O10, Cu4 I6'
_chemical_formula_sum            'C22 H48 Ba Cu4 I6 O10'
_chemical_formula_weight         1625.57
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-07-25
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 113.340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.793(2)
_cell_length_b                   15.1720(10)
_cell_length_c                   17.927(2)
_cell_measurement_reflns_used    6673
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.5093
_cell_measurement_theta_min      3.1826
_cell_volume                     4443.5(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.4678
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.087
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32684
_diffrn_reflns_theta_full        26.597
_diffrn_reflns_theta_max         29.508
_diffrn_reflns_theta_min         3.394
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.964
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.76
_refine_diff_density_min         -2.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         10718
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.0005826
_refine_ls_shift/su_mean         0.0000240
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 849. 0.114E+04 608. 159. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1602
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1602
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6797
_reflns_number_total             10718
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.38
_oxford_diffrn_Wilson_scale      4.97
_oxford_refine_ls_r_factor_ref   0.1221
_oxford_refine_ls_scale          0.7372(14)
_oxford_reflns_number_all        10718
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smrb32 in P 1 21/n 1'
_cod_data_source_file            ic501963y_si_007.cif
_cod_data_source_block           global
_cod_depositor_comments
'Adding full bibliography for 4341352--4341362.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C22 H48 Ba1 Cu4 I6 O10'
_cod_database_code               4341352
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) H   (  13,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) H   ( 163,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = C(17) TO C(18) 
U(IJ)'S  0.0, 0.010000 = C(17) TO C(19) 
U(IJ)'S  0.0, 0.010000 = O(6) TO C(11) 
U(IJ)'S  0.0, 0.010000 = O(5) TO C(10) 
U(IJ)'S  0.0, 0.010000 = O(10) TO C(20) 
END                                                                             
;