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_7206833
_publ_section_title
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 Zinc(ii) coordination polymers with pseudopeptidic ligands
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_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
'C64 H104 Br N16 O8 Zn3, Br5, 6(C2 H6 O), 7(H2 O)'
_chemical_formula_sum            'C76 H154 Br6 N16 O21 Zn3'
_chemical_formula_weight         2303.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 123.780(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   39.030(2)
_cell_length_b                   11.8817(2)
_cell_length_c                   27.6330(13)
_cell_measurement_reflns_used    21281
_cell_measurement_temperature    173
_cell_measurement_theta_max      73.6456
_cell_measurement_theta_min      1.9219
_cell_volume                     10651.2(12)
_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
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42529
_diffrn_reflns_theta_full        72.50
_diffrn_reflns_theta_max         73.81
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.972
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
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    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             4760
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
SQUEEZE suggests 891 e/cell = 223 e/asu
Solvent mixture was EtOH/H2O, and before SQUEEZE the ratio looked to be
roughly 1:1
EtOH = C2H6O = 26e. H2O = 10e
6EtOH . 7H2O = 226e so this was used as the solvent present

The protons of the N1/N14/N21/N34/N41/N54/N61/N74 NH2 groups and the
N4/N11/N24/N31/N44/N51/N64/N71 NH groups were not located, so the asu
is low by H24.

Thus asu is low by 6(C2H6O) + 7(H2O) + H24 = (C12H36O6) + (H14O7) + H24
= C12 H74 O13, and the UNIT low by C48 H296 O52,
i.e. C256 H320 N64 O32 Zn12 Br24
;
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 7224 Friedel pairs'
_refine_ls_abs_structure_Flack   0.004(15)
_refine_ls_extinction_coef       0.000029(6)
_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   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         18211
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0668P)^2^+16.2469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                16436
_reflns_number_total             18211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05872j.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      C2
_cod_database_code               7206833