Copper pyromellitates: a complex story
Clegg, William; Holcroft, James M.; Martin, Nicola C.; CrystEngComm 17 (2015) 2857–; doi:10.1039/C5CE00470E

data_7219782
_publ_section_title
;
 Copper pyromellitates: a complex story
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2857
_journal_paper_doi               10.1039/C5CE00470E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'2 N H4 +,Cu N4 H12 2+, 2 C10 H11 Cu N3 O8 2-,2H2 O'
_chemical_formula_sum            'C20 H46 Cu3 N12 O18'
_chemical_formula_weight         933.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.371(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2343(7)
_cell_length_b                   19.5788(16)
_cell_length_c                   10.9336(9)
_cell_measurement_reflns_used    4625
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.72
_cell_volume                     1733.9(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'narrow-frame \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11979
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.667
_diffrn_reflns_theta_min         2.080
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.917
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             962
_exptl_crystal_recrystallization_method
'Obtained direct from slow diffusion synthesis'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+3.5743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3125
_reflns_number_total             3952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00470e2.cif
_cod_data_source_block           wc19
_cod_depositor_comments
'Adding full bibliography for 7219775--7219784.cif.'
_cod_database_code               7219782
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.626
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              31387