A second polymorph of <i>cyclo</i>-tetrakis{μ~2~-[(dimethylamino)methyl]phenyl-κ^3^<i>C</i>^2^:<i>C</i>^2^,<i>N</i>}copper tetrahydrofuran solvate
Tooke, Duncan M.; Lutz, Martin; Spek, Anthony L.; Acta Crystallographica Section E 61 (2005) m1245–m1247; doi:10.1107/S1600536805016685

data_2206015
_publ_section_title
;A second polymorph of
 <i>cyclo</i>-tetrakis{\m~2~-[(dimethylamino)methyl]phenyl-\k^3^<i>C</i>^2^:<i>C</i>^2^,<i>N</i>}copper
 tetrahydrofuran solvate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1245
_journal_page_last               m1247
_journal_paper_doi               10.1107/S1600536805016685
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Cu4 (C9 H12 N)4] , C4 H8 O'
_chemical_formula_moiety         'C36 H48 Cu4 N4 , C4 H8 O'
_chemical_formula_sum            'C40 H56 Cu4 N4 O'
_chemical_formula_weight         863.05
_chemical_name_common
;
cyclo-tetrakis{\m~2~-[(dimethylamino)methyl]phenyl-\k^3^C^2^:C^2^,N}copper
tetrahydrofuran solvate
;
_chemical_name_systematic
;
cyclo-tetrakis{\m~2~-[(dimethylamino)methyl]phenyl-\k^3^C^2^:C^2^,N}copper
tetrahydrofuran solvate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4952(2)
_cell_length_b                   13.2026(3)
_cell_length_c                   31.5269(6)
_cell_measurement_reflns_used    64686
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.29
_cell_volume                     3952.25(14)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        DENZO
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            53905
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.158
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Blessing, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.26
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   -0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9022
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0187
_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^)+(0.0157P)^2^+1.2769P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                8758
_reflns_number_total             9022
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6430.cif
_cod_data_source_block           I
_cod_database_code               2206015
_cod_database_fobs_code          2206015