Reactivity of the Verdoheme Analogues. Opening of the Planar Macrocycle by Amide and Thiolate Nucleophiles To Form Helical Complexes
James A. Johnson; Marilyn M. Olmstead; Alan L. Balch; Inorganic Chemistry 38 (1999) 5379–5383; doi:10.1021/ic9904283

data_4322392
_publ_section_title
;
 Reactivity of the Verdoheme Analogues. Opening of the Planar Macrocycle
 by Amide and Thiolate Nucleophiles To Form Helical Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5379
_journal_page_last               5383
_journal_paper_doi               10.1021/ic9904283
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C36 H46 N4 O S Zn'
_chemical_formula_weight         648.20
_chemical_name_common            Zn(OEBSMe)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.85(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.134(3)
_cell_length_b                   16.819(4)
_cell_length_c                   14.848(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      4.1
_cell_volume                     3359.8(13)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL PLUS V. 5.02, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Syntex P2~1~'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.1676
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6016
_diffrn_reflns_theta_full        64.00
_diffrn_reflns_theta_max         64.00
_diffrn_reflns_theta_min         3.78
_diffrn_standards_decay_%        3.5
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  0.9133
_exptl_absorpt_correction_T_min  0.4902
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2: an empirical absorption correction program. Parkin, S.; Moezzi,
 B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1891
_refine_ls_R_factor_gt           0.1016
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+20.4100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2407
_refine_ls_wR_factor_ref         0.2866
_reflns_number_gt                3080
_reflns_number_total             5573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9904283_1.cif
_cod_data_source_block           mn843
_cod_database_code               4322392