Hydrothermal crystal engineering using hard and soft acids and bases: synthesis and X-ray crystal structures of the metal hydroxide-based phases M3M′2(OH)2[NC5H3(CO2)2-2,4]4(H2O)4 (M = Co, Ni, Zn; M′ = Pd, Pt)
Gerrard, Lee A.; Wood, Paul T.; Chemical Communications  (2000) 2107–; doi:10.1039/b006094l

data_7111083
_publ_section_title
;
 Hydrothermal crystal engineering using hard and soft acids and bases:
 synthesis and X-ray crystal structures of the metal hydroxide-based
 phases M3M&#x2032;2(OH)2[NC5H3(CO2)2-2,4]4(H2O)4 (M = Co, Ni, Zn;
 M&#x2032; = Pd, Pt)
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2107
_journal_paper_doi               10.1039/b006094l
_journal_year                    2000
_chemical_compound_source        'Hydrothermal synthesis'
_chemical_formula_moiety         'Pd2 Zn3 C28 H22 N4 O22'
_chemical_formula_sum            'C28 H22 N4 O22 Pd2 Zn3'
_chemical_formula_weight         1175.41
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL and manual editing'
_cell_angle_alpha                75.94(3)
_cell_angle_beta                 88.73(3)
_cell_angle_gamma                84.78(3)
_cell_formula_units_Z            1
_cell_length_a                   6.529(1)
_cell_length_b                   8.124(2)
_cell_length_c                   16.719(3)
_cell_measurement_temperature    293(2)
_cell_volume                     856.7(3)
_computing_cell_refinement
'DENZO AND SCALEPACK (Otwinowski and Minor, 1985)'
_computing_data_collection       'MSC Raxis II control software'
_computing_data_reduction        'SHELX97-SHELXPRO (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL+XP
_computing_publication_material  SHELXTL+XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku R-axis IIc'
_diffrn_measurement_method       'image plate oscillation photographs'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5386
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    3.202
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yelow
_exptl_crystal_density_diffrn    2.278
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.733
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.976
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         2858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.225
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_obs          0.0412
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1348
_refine_ls_wR_factor_obs         0.1000
_reflns_number_observed          2165
_reflns_number_total             2862
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006094lsup1.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'n/a' was changed to '?' - the value
is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111083