Control of molecular architecture by the degree of deprotonation: self-assembled di- and tetranuclear copper(II) complexes of N,N'-bis(2-pyridylmethyl)pyrazine-2,3-dicarboxamide
Hausmann, Julia; Jameson, Geoffrey B.; Brooker, Sally; Chemical Communications (Cambridge, United Kingdom)  (2003) 2992–2993; doi:10.1039/b308263f

data_7113599
_publ_section_title
;
 Control of molecular architecture by the degree of deprotonation:
 self-assembled di- and tetranuclear copper(II) complexes of
 N,N'-bis(2-pyridylmethyl)pyrazine-2,3-dicarboxamide
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   24
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2992
_journal_page_last               2993
_journal_paper_doi               10.1039/b308263f
_journal_year                    2003
_chemical_formula_sum            'C79 H70.5 B4 Cu4 F16 N27.5 O8'
_chemical_formula_weight         2134.53
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.189(3)
_cell_length_b                   15.191(3)
_cell_length_c                   20.048(4)
_cell_measurement_reflns_used    18861
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      1.67
_cell_volume                     4625.7(16)
_computing_cell_refinement       'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_data_collection       'WinXpose 1.05 (Stoe & Cie GmbH, 2000)'
_computing_data_reduction        'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_molecular_graphics    'XP: SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_publication_material  'XCIF: SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_refinement  'XL: SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_solution    'XS: SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24008
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.9076
_exptl_absorpt_correction_T_min  0.8183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-RED 1.22 (Stoe & Cie GmbH, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       0.0528(15)
_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   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1290
_refine_ls_number_reflns         15222
_refine_ls_number_restraints     1487
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1176P)^2^+10.6145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1952
_refine_ls_wR_factor_ref         0.2204
_reflns_number_gt                12059
_reflns_number_total             15222
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103902
_cod_data_source_file            b308263f.txt
_cod_data_source_block           cul3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4625.8(16)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7113599