Hydrothermal synthesis and structural characterisation of [H2DABCO]3[Cu16Cl22]: a new copper(i) chloride framework
Williams, Edward R.; Weller, Mark T.; CrystEngComm 15 (2013) 31–; doi:10.1039/c2ce26068a

data_7208876
_publ_section_title
;
 Hydrothermal synthesis and structural characterisation of
 [H2DABCO]3[Cu16Cl22]: a new copper(i) chloride framework
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              31
_journal_paper_doi               10.1039/c2ce26068a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C18 H42 Cl22 Cu16 N6'
_chemical_formula_weight         2139.12
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-06-01 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8722(5)
_cell_length_b                   12.9237(4)
_cell_length_c                   29.641(2)
_cell_measurement_reflns_used    22503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4931.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
Number of images: 104
Slice: -110.0000 - -6.0000
Image width: 1.0000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: -15.0000
Phi: 225.0000
XTD: 44.7940
2theta: -19.6237
scan:
Number of images: 98
Slice: -58.0000 - 40.0000
Image width: 1.0000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 70.0000
Phi: 0.0000
XTD: 44.7940
2theta: -19.6237

;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_orient_matrix_UB_11      -0.025923
_diffrn_orient_matrix_UB_12      -0.069112
_diffrn_orient_matrix_UB_13      0.010170
_diffrn_orient_matrix_UB_21      -0.067349
_diffrn_orient_matrix_UB_22      0.032216
_diffrn_orient_matrix_UB_23      0.009245
_diffrn_orient_matrix_UB_31      -0.028765
_diffrn_orient_matrix_UB_32      -0.013146
_diffrn_orient_matrix_UB_33      -0.030810
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_unetI/netI     0.057
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            23612
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    7.962
_exptl_absorpt_correction_T_max  0.5032
_exptl_absorpt_correction_T_min  0.3814
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.769
_refine_diff_density_min         -2.663
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         11287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+135.5673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                10304
_reflns_number_total             11287
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2ce26068a.txt
_cod_data_source_block           2012erw042_at1
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7208876