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_7013282
_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 H2 N3 O -)2, H2 O, H2 O'
_chemical_formula_structural     '{[Cu((NC)2CCONH2)2(OH2)] * H2O}'
_chemical_formula_sum            'C8 H8 Cu N6 O4'
_chemical_formula_weight         315.74
_chemical_name_common            '((Cu(cdc)!2$(OH!2$)) * H!2$O)!\\infty$'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2003-05-19T13:28:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                77.727(4)
_cell_angle_beta                 80.513(4)
_cell_angle_gamma                74.160(6)
_cell_formula_units_Z            2
_cell_length_a                   7.2230(5)
_cell_length_b                   7.4380(5)
_cell_length_c                   11.5910(11)
_cell_measurement_reflns_used    9269
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     581.59(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w rotations'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.1135273
_diffrn_orient_matrix_UB_12      -0.0344702
_diffrn_orient_matrix_UB_13      -0.0832873
_diffrn_orient_matrix_UB_21      -0.0878271
_diffrn_orient_matrix_UB_22      -0.111014
_diffrn_orient_matrix_UB_23      -0.0125558
_diffrn_orient_matrix_UB_31      -0.0377672
_diffrn_orient_matrix_UB_32      0.0565264
_diffrn_orient_matrix_UB_33      -0.0573202
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9744
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.9
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2661
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+1.2192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                2397
_reflns_number_total             2661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306169h.txt
_cod_data_source_block           k01prr22
_cod_original_formula_sum        'C8 H8 Cu1 N6 O4'
_cod_database_code               7013282
_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. All other hydrogen atoms are modelled as riding with
SHELXL standard parameters for bondlengths, -angles and thermal factors.
;