Synthesis, crystal structure and disorder–order phase transition of a new diamine templated metal sulfate, (C3H12N2)2[Cu(H2O)4(SO4)2](HSO4)2
Chen, Chun-Hong; Mu, Rong; Zhang, Li; Xu, Guan-Cheng; CrystEngComm 18 (2016) 2719–; doi:10.1039/C5CE02442K

data_7224574
_publ_section_title
;
 Synthesis, crystal structure and disorder--order phase transition of a
 new diamine templated metal sulfate, (C3H12N2)2[Cu(H2O)4(SO4)2](HSO4)2
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2719
_journal_paper_doi               10.1039/C5CE02442K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C6 H34 Cu N4 O20 S4'
_chemical_formula_weight         674.15
_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
_audit_update_record
;
2016-01-20 deposited with the CCDC.
2016-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                94.771(4)
_cell_angle_beta                 100.757(4)
_cell_angle_gamma                95.748(4)
_cell_formula_units_Z            2
_cell_length_a                   10.649(4)
_cell_length_b                   10.677(4)
_cell_length_c                   10.799(4)
_cell_measurement_reflns_used    7560
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5142
_cell_measurement_theta_min      2.4661
_cell_volume                     1193.7(8)
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9604
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.7724
_exptl_absorpt_correction_T_min  0.7538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.311
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0486P)^2^+0.7849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                3991
_reflns_number_total             4242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02442k2.cif
_cod_data_source_block           ee
_cod_depositor_comments
'Adding full bibliography for 7224573--7224574.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7224574