<i>catena</i>-Poly[[[iodidocopper(I)]-{μ-<i>N</i>-[(pyridin-2-yl-κ<i>N</i>)methylidene]pyridin-3-amine-κ^2^<i>N</i>^3^:<i>N</i>^1^}] acetonitrile hemisolvate]
Mahmoudi, Ali; Dehghanpour, Saeed; Babakhodaverdi, Mojtaba; Acta Crystallographica Section E 68 (2012) m1277–m1278; doi:10.1107/S1600536812037270

data_2236628
_publ_section_title
;
 <i>catena</i>-Poly[[[iodidocopper(I)]-{\m-<i>N</i>-[(pyridin-2-yl-\k<i>N</i>)methylidene]pyridin-3-amine-\k^2^<i>N</i>^3^:<i>N</i>^1^}]
 acetonitrile hemisolvate]
;
_journal_coeditor_code           SU2480
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1277
_journal_page_last               m1278
_journal_paper_doi               10.1107/S1600536812037270
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu I (C11 H9 N3)], 0.5C2 H3 N'
_chemical_formula_moiety         'C22 H9 Cu1 I1 N3, 0.5(C2 H3 N)'
_chemical_formula_sum            'C12 H13.5 Cu I N3'
_chemical_formula_weight         394.18
_chemical_name_systematic
;
<i>catena</i>-Poly[[[iodidocopper(I)]-{\m-<i>N</i>-[(pyridin-2-
yl-\k<i>N</i>)methylidene]pyridin-3-amine-\k^2^<i>N</i>^3^:<i>N</i>^1^}]
acetonitrile monosolvate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.741(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.1800(2)
_cell_length_b                   13.2303(7)
_cell_length_c                   27.9383(13)
_cell_measurement_reflns_used    19063
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2653.7(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.104
_diffrn_reflns_av_sigmaI/netI    0.096
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            19063
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly acetonitrile).
Attempts made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there were
solvent cavities with a total volume of 196 \%A^3^ containing
approximately 60 electrons per unit cell.
In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
_refine_diff_density_max         1.388
_refine_diff_density_min         -1.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0943P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1778
_reflns_number_gt                2627
_reflns_number_total             4676
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2480.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C12 H13.5 Cu1 I1 N3'
_cod_database_code               2236628
_cod_database_fobs_code          2236628