Probing the Nature of the CoIII Ion in Corrins: The Structural and Electronic Properties of Dicyano- and Aquacyanocobyrinic Acid Heptamethyl Ester and a Stable Yellow Dicyano- and Aquacyanocobyrinic Acid Heptamethyl Ester
Susan M. Chemaly; Kenneth L. Brown; Manuel A. Fernandes; Orde Q. Munro; Craig Grimmer; Helder M. Marques; Inorganic Chemistry 50 (2011) 8700–8718; doi:10.1021/ic200285k

data_4326204
_publ_section_title
;
 Probing the Nature of the CoIII Ion in Corrins: The Structural and
 Electronic Properties of Dicyano- and Aquacyanocobyrinic Acid Heptamethyl
 Ester and a Stable Yellow Dicyano- and Aquacyanocobyrinic Acid
 Heptamethyl Ester
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8700
_journal_page_last               8718
_journal_paper_doi               10.1021/ic200285k
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety
;
C53 H71 Co N6 O15, C H4 O, H2 O
;
_chemical_formula_sum            'C54 H77 Co N6 O17'
_chemical_formula_weight         1141.15
_chemical_name_systematic
;
 ?
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4852(4)
_cell_length_b                   18.9342(8)
_cell_length_c                   31.3583(13)
_cell_measurement_reflns_used    3467
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.02
_cell_measurement_theta_min      2.23
_cell_volume                     5631.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1143
_diffrn_reflns_av_sigmaI/netI    0.1377
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            35872
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       plate
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         10493
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                6318
_reflns_number_total             10493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200285k_si_002.cif
_cod_data_source_block           9m_sc1_0f
_cod_database_code               4326204