Zinc(ii) coordination polymers with pseudopeptidic ligands
Martí-Centelles, Vicente; Kumar, D. Krishna; White, Andrew J. P.; Luis, Santiago V.; Vilar, Ramon; CrystEngComm 13 (2011) 6997–; doi:10.1039/c1ce05872j

data_7206830
_publ_section_title
;
 Zinc(ii) coordination polymers with pseudopeptidic ligands
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              6997
_journal_paper_doi               10.1039/c1ce05872j
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C24 H30 N4 O4 Zn, S O4, 2.25(H2 O), 0.5(C2 H6 O)'
_chemical_formula_sum            'C25 H37.5 N4 O10.75 S Zn'
_chemical_formula_weight         663.52
_chemical_name_systematic
;
?
;
_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            8
_cell_length_a                   13.9923(2)
_cell_length_b                   14.3096(2)
_cell_length_c                   32.6979(5)
_cell_measurement_reflns_used    32493
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.3815
_cell_measurement_theta_min      3.1088
_cell_volume                     6546.91(16)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            65807
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         32.46
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
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            Colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
SQUEEZE suggests 244 e/cell = 30.5 e/asu
Solvent used was EtOH/H2O mixture. Before SQUEEZE, some H2O was identified.
The rest was highly disordered, but looked most like ethanol.
EtOH = C2H6O = 26e
1.17EtOH = 30.4e. This was rounded down to 1EtOH for simplicity.

The protons of the N1/N14 NH2 groups, the N4/N11 NH groups, and the
O29/O30 and O61-O65 H2O groups were not located. The asu is thus H29 low.

The asu is thus (C2 H6 O) + H29 low = C2 H35 O low.
So the UNIT is C8 H140 O4 low, i.e. C192 H160 N32 O82 S8 Zn8
;
_refine_diff_density_max         1.221
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 9664 Friedel pairs'
_refine_ls_abs_structure_Flack   0.043(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         21753
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+7.6726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                17574
_reflns_number_total             21753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05872j.txt
_cod_data_source_block           4
_cod_depositor_comments
;
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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        'C25 H37.50 N4 O10.75 S Zn'
_cod_database_code               7206830