Heptaaquatetra-μ~3~-hydroxy-hexa-μ~2~-<small>L</small>-leucine-(<small>L</small>-leucine)tetraytterbium(III) tetrachlorozinc(II) trichlorohydroxyzinc(II) tetrachloride octahydrate
Jinping Wang; Chunji Niu; Ninghai Hu; Acta Crystallographica Section C 60 (2004) m143–m146; doi:10.1107/S0108270104002264

data_2013746
_publ_section_title
;Heptaaquatetra-\m~3~-hydroxy-hexa-\m~2~-<small>L</small>-leucine-(<small>L</small>-leucine)tetraytterbium(III)
 tetrachlorozinc(II) trichlorohydroxyzinc(II) tetrachloride octahydrate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m143
_journal_page_last               m146
_journal_paper_doi               10.1107/S0108270104002264
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'[Yb4 (O H)4 (C6 H13 N O2)7 (H2 O)7] [Zn Cl4] [Zn Cl3 (O H)] Cl4, 8H2 O'
_chemical_formula_moiety
'C42 H110 N7 O25 Yb4, Cl3 O Zn 2+, Cl4 Zn 2+, 4Cl 1-, 8H2 O'
_chemical_formula_sum            'C42 H126 Cl11 N7 O34 Yb4 Zn2'
_chemical_formula_weight         2486.35
_chemical_name_systematic
;Heptaaquatetra-\m~3~-hydroxy-hexa-\m~2~-L-leucine-(L-leucine)tetraytterbium(III)
tetrachloratezinc(II)
 trichlorohydroxyzinc(II) tetrachloride octahydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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                   18.171(4)
_cell_length_b                   22.130(5)
_cell_length_c                   23.251(7)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.36
_cell_measurement_theta_min      5.20
_cell_volume                     9350(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.025
_diffrn_reflns_av_sigmaI/netI    0.139
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            10699
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.851
_exptl_absorpt_correction_T_max  0.5855
_exptl_absorpt_correction_T_min  0.4395
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(SHELXTL; Siemens, 1994)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             4904
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.925
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   '-0.013(15) - 385 Friedel pairs'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         10247
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.01P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                5857
_reflns_number_total             10247
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1556.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-11-30

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (12 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_bond_publ_flag'
value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (12 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        9349(4)
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_database_code               2013746
_cod_database_fobs_code          2013746