Low-dimensional compounds containing cyano groups. IV. Bis(2,2'-bipyridine-κ^2^<i>N</i>,<i>N</i>^1^)(dicyanamido-κ<i>N</i>')copper(II) perchlorate and μ-dicyanamido-κ^2^<i>N</i>^1^:<i>N</i>^5^-bis[bis(2,2'-bipyridine-κ^2^<i>N</i>,<i>N</i>')copper(II)] triperchlorate ethanol hemisolvate, complexes with unusual dicyanamide coordination
Potočňák, Ivan; Burčák, Milan; Massa, Werner; Jäger, Lothar; Acta Crystallographica Section C 58 (2002) m523–m528; doi:10.1107/S0108270102015731

data_2012966
_publ_section_title
;Low-dimensional compounds containing cyano groups. IV.
 Bis(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>^1^)(dicyanamido-\k<i>N</i>')copper(II)
 perchlorate and
 \m-dicyanamido-\k^2^<i>N</i>^1^:<i>N</i>^5^-bis[bis(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')copper(II)]
 triperchlorate ethanol hemisolvate, complexes with unusual dicyanamide
 coordination
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m523
_journal_page_last               m528
_journal_paper_doi               10.1107/S0108270102015731
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
'[Cu2 (C10 H8 N2)4 (C2 N3)] (Cl O4)3 , 0.5C2 H6 O'
_chemical_formula_moiety         'C42 H32 N11 Cu2 3+ , 3Cl O4 - , 0.5C2 H6 O'
_chemical_formula_sum            'C43 H35 Cl3 Cu2 N11 O12.5'
_chemical_formula_weight         1139.25
_chemical_name_systematic
;
\m-dicyanamido-\k^2^N^1^:N^3^-bis[bis(2,2'-bipyridine-\k^2^N,N')copper(II)]
tris(perchlorate) ethanol hemisolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                74.120(10)
_cell_angle_beta                 83.371(11)
_cell_angle_gamma                80.046(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2999(9)
_cell_length_b                   14.3808(12)
_cell_length_c                   16.4311(16)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.25
_cell_volume                     2299.7(4)
_computing_cell_refinement       'CELL in IPDS'
_computing_data_collection       'EXPOSE in IPDS (Stoe, 1999)'
_computing_data_reduction        'INTEGRATE in IPDS'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Stoe IPDS image-plate'
_diffrn_measurement_method       'D = 60mm, \f 0-250\%, \D\f 1.6\%, 2 min/rec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_sigmaI/netI    0.108
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27918
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'indexed faces'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10314
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.104
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0564P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.099
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                5455
_reflns_number_total             10314
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1508.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C43 H35 Cl3 Cu2 N11 O12.50'
_cod_database_code               2012966
_cod_database_fobs_code          2012966