The synthesis of a corrole analogue of aquacobalamin (vitamin b12a) and its ligand substitution reactions.
Zipp, Caitlin F.; Michael, Joseph P.; Fernandes, Manuel A.; Mathura, Sadhna; Perry, Christopher B.; Navizet, Isabelle; Govender, Penny P.; Marques, Helder M.; Inorganic chemistry 53 (2014) 4418–4429; doi:10.1021/ic5000793

data_4338110
_publ_section_title
;
 The synthesis of a corrole analogue of aquacobalamin (vitamin b12a) and
 its ligand substitution reactions.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4418
_journal_page_last               4429
_journal_paper_doi               10.1021/ic5000793
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C23 H19 Cl2 N O3'
_chemical_formula_sum            'C23 H19 Cl2 N O3'
_chemical_formula_weight         428.29
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_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            16
_cell_length_a                   38.968(4)
_cell_length_b                   46.919(5)
_cell_length_c                   4.3266(3)
_cell_measurement_reflns_used    346
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.08
_cell_measurement_theta_min      3.25
_cell_volume                     7910.5(13)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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
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_diffrn_reflns_av_sigmaI/netI    0.3312
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            7363
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       needle
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.32(12)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4217
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.715
_refine_ls_R_factor_all          0.2176
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                1332
_reflns_number_total             4217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5000793_si_003.cif
_cod_data_source_block           11c_czhmm25_0s
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338110--4338111.cif.
;
_cod_original_cell_volume        7910.6(13)
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               4338110