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

data_7219781
_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         '4 C6 H16 N +,C22 H12 Cu2 O18 4-,2 C H4 O'
_chemical_formula_sum            'C48 H84 Cu2 N4 O20'
_chemical_formula_weight         1164.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                78.671(2)
_cell_angle_beta                 64.251(2)
_cell_angle_gamma                71.747(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5053(11)
_cell_length_b                   11.5543(11)
_cell_length_c                   12.0160(11)
_cell_measurement_reflns_used    8941
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      29.11
_cell_measurement_theta_min      2.55
_cell_volume                     1362.9(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL and local programs'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'narrow-frame \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11335
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.126
_diffrn_reflns_theta_min         1.886
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             618
_exptl_crystal_recrystallization_method
'Obtained direct from slow diffusion synthesis'
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.240
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0043(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6487
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+2.2682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5709
_reflns_number_total             6487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00470e2.cif
_cod_data_source_block           wc5
_cod_depositor_comments
'Adding full bibliography for 7219775--7219784.cif.'
_cod_database_code               7219781
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.684
_shelx_estimated_absorpt_t_max   0.821
_shelx_res_checksum              15178