Conformationally-locked metallomacrocycles—prototypes for a novel type of axial chirality
Chow, Hoi Shan; Constable, Edwin C.; Frantz, Richard; Housecroft, Catherine E.; Lacour, Jérôme; Neuburger, Markus; Rappoport, Dmitrij; Schaffner, Silvia; New Journal of Chemistry 33 (2009) 376–; doi:10.1039/b819588a

data_7053774
_publ_section_title
;
 Conformationally-locked metallomacrocycles---prototypes for a novel type
 of axial chirality
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              376
_journal_paper_doi               10.1039/b819588a
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C52 H50 Fe N6 O8, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C54 H53 F12 Fe N7 O8 P2'
_chemical_formula_weight         1273.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-12-08
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                90
_cell_angle_beta                 92.9257(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2659(1)
_cell_length_b                   14.8059(1)
_cell_length_c                   20.5792(2)
_cell_measurement_reflns_used    27885
_cell_measurement_temperature    173
_cell_measurement_theta_max      29
_cell_measurement_theta_min      1
_cell_volume                     5558.25(7)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54042
_diffrn_reflns_theta_full        28.690
_diffrn_reflns_theta_max         28.690
_diffrn_reflns_theta_min         1.695
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1195
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         8366
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.025578
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^
Method = SHELXL 97 (Sheldrick, 1997)
W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ]
P(i) are:
0.00 0.756E-01 0.00 0.00 0.00 0.333
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0660
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0574
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                8366
_reflns_number_total             14324
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.1958(3)
_oxford_structure_analysis_title '12080937 hsc121_2_173k'
_cod_data_source_file            b819588asup1.cif
_cod_data_source_block           hsc121_173k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C54 H53 F12 Fe1 N7 O8 P2'
_cod_database_code               7053774