Complexes of hexamethylenetetramine with zinc-tetraarylporphyrins, and their assembly modes in crystals as clathrates and hydrogen-bonding network polymers
Israel Goldberg; Mikki Vinodu; New J.Chem.(Nouv.J.Chim.)  (2004) –; doi:

data_7050351
_publ_section_title
;
Complexes of hexamethylenetetramine with
zinc-tetraarylporphyrins, and their assembly modes in crystals as
clathrates and hydrogen-bonding network polymers
;
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'
_journal_year                    2004
_chemical_formula_moiety
'(C48 H28 N4 O8 Zn), 2(C6 H12 N4), 2(C9 H10 O2)'
_chemical_formula_sum            'C78 H72 N12 O12 Zn'
_chemical_formula_weight         1434.85
_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
_cell_angle_alpha                76.002(2)
_cell_angle_beta                 89.056(3)
_cell_angle_gamma                82.936(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3600(4)
_cell_length_b                   11.4980(6)
_cell_length_c                   15.3610(8)
_cell_measurement_reflns_used    6025
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.39
_cell_volume                     1761.81(15)
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & Omega 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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14853
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             750
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         8125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0988P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1513
_reflns_number_gt                6025
_reflns_number_total             8125
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               7050351