Structural characterisation of a water intercalated bis-amide tecton and copper promoted monohydration of a dinitrile
Bjernemose, Jens K.; McKenzie, Christine J.; Raithby, Paul R.; Teat, Simon J.; Dalton Transactions  (2003) 2639–; doi:10.1039/b306169h

data_7013283
_publ_section_title
;
 Structural characterisation of a water intercalated bis-amide tecton
 and copper promoted monohydration of a dinitrile
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              2639
_journal_paper_doi               10.1039/b306169h
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Cu 2+,  (C4 H4 N3 O2 -)2, H2 O'
_chemical_formula_structural     '[Cu ((OCNH2)2CCN)2] * H2O'
_chemical_formula_sum            'C8 H10 Cu N6 O5'
_chemical_formula_weight         333.76
_chemical_name_common            '(Cu(cyma)!2$) * H!2$O'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-05-19T15:55:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.065(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5923(5)
_cell_length_b                   11.2749(7)
_cell_length_c                   12.5768(8)
_cell_measurement_reflns_used    3031
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      5.97
_cell_measurement_wavelength     0.6893
_cell_volume                     1170.83(12)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.96
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device_type  'Bruker AXS SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6893
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4025
_diffrn_reflns_theta_full        28.57
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Daresbury SRS Station 9.8'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.899
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1579
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+1.1221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                1472
_reflns_number_total             1579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306169h.txt
_cod_data_source_block           bath33
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7013283
_refine_ls_hydrogen_treatment_special
;
All hydrogens on hetero atoms are unless otherwise stated located from the
Fourier difference map and in the refinement restrained to have bondlengths
of 1.00(1)\%A. Their thermal factors are set to 1.2*U~iso~ of the atom on
which they are riding.
;