Di-μ-chlorido-bis{bis[4-(adamantan-1-ylcarbamoyl)pyridine-κ<i>N</i>]chloridocopper(II)} hemihydrate
Wang, Ying-Chun; Acta Crystallographica Section E 68 (2012) m147–; doi:10.1107/S1600536812000670

data_2233509
_publ_section_title
;
 Di-\m-chlorido-bis{bis[4-(adamantan-1-ylcarbamoyl)pyridine-\k<i>N</i>]chloridocopper(II)}
 hemihydrate
;
_journal_coeditor_code           HY2504
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m147
_journal_paper_doi               10.1107/S1600536812000670
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu2 Cl4 (C16 H20 N2 O)4], 0.5H2 O'
_chemical_formula_moiety         'C64 H80 Cl4 Cu2 N8 O4, 0.5(H2 O)'
_chemical_formula_sum            'C64 H81 Cl4 Cu2 N8 O4.5'
_chemical_formula_weight         1303.25
_chemical_name_systematic
;
Di-\m-chlorido-bis{bis[4-(adamantan-1-ylcarbamoyl)pyridine-
\k<i>N</i>]chloridocopper(II)} hemihydrate
;
_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           SHELXL-97
_cell_angle_alpha                92.221(6)
_cell_angle_beta                 95.993(8)
_cell_angle_gamma                96.727(9)
_cell_formula_units_Z            1
_cell_length_a                   6.739(4)
_cell_length_b                   11.149(6)
_cell_length_c                   21.814(12)
_cell_measurement_reflns_used    4355
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.56
_cell_volume                     1616.6(16)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics
'XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury2 CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16110
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.8798
_exptl_absorpt_correction_T_min  0.7791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             683
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.768
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+0.8170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1793
_refine_ls_wR_factor_ref         0.1968
_reflns_number_gt                4988
_reflns_number_total             6320
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2504.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C64 H81 Cl4 Cu2 N8 O4.50'
_cod_database_code               2233509
_cod_database_fobs_code          2233509