Crystal-to-crystal transformation upon dehydration of a copper(II) 2,2':6',2''-terpyridine complex
Schmitt, Laurette; Labat, Gaël; Stoeckli-Evans, Helen; Acta Crystallographica Section C 66 (2010) m343–m347; doi:10.1107/S0108270110041090

data_2017820
_publ_section_title
;
 Crystal-to-crystal transformation upon dehydration of a copper(II)
 2,2':6',2''-terpyridine complex
;
_journal_coeditor_code           GA3158
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m343
_journal_page_last               m347
_journal_paper_doi               10.1107/S0108270110041090
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Cu (C15 H11 N3) Cl (H2 O)] [Cu (C15 H11 N3) (S2 O6) Cl] , 2H2 O'
_chemical_formula_moiety
'C15 H13 Cl Cu N3 O, C15 H11 Cl Cu N3 O6 S2, 2(H2 O)'
_chemical_formula_sum            'C30 H28 Cl2 Cu2 N6 O9 S2'
_chemical_formula_weight         878.68
_chemical_name_systematic
;
[aquachlorido(2,2':6',2''-terpyridyl-\k^3^N,N',N'')]copper(II)
[chlorido(2,2':6',2''-terpyridyl-\k^3^N,N',N'')(dithionato-\kO)]cuprate(II)
dihydrate
;
_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                83.096(10)
_cell_angle_beta                 82.870(11)
_cell_angle_gamma                73.675(11)
_cell_formula_units_Z            2
_cell_length_a                   8.0705(10)
_cell_length_b                   8.5890(10)
_cell_length_c                   25.177(3)
_cell_measurement_reflns_used    33786
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      1.64
_cell_volume                     1655.2(4)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2006)'
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       '\f and \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  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            25099
_diffrn_reflns_theta_full        29.28
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS in PLATON; Spek, 2009)'
_exptl_crystal_colour            emerald-green
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.950
_refine_diff_density_min         -1.474
_refine_ls_extinction_coef       0.0042(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8888
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0646P)^2^+0.8251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                8053
_reflns_number_total             8888
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3158.cif
_cod_data_source_block           I
_cod_original_cell_volume        1655.2(3)
_cod_database_code               2017820
_cod_database_fobs_code          2017820