Formation of a [1???+???1] metallomacrocycle from a heterotritopic ligand containing two terpy and one bipy metal-binding domains
Smith, Christopher B.; Constable, Edwin C.; Housecroft, Catherine E.; Kariuki, Benson M.; Chemical Communications  (2002) 2068–; doi:10.1039/b205233d

data_7114047
_publ_section_title
;
 Formation of a [1???+???1] metallomacrocycle from a heterotritopic ligand
 containing two terpy and one bipy metal-binding domains
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2068
_journal_paper_doi               10.1039/b205233d
_journal_year                    2002
_chemical_formula_moiety         'C64 H58 Fe N8 O8, C3 H6 O, 2(P F6) '
_chemical_formula_sum            'C67 H64 F12 Fe N8 O9 P2'
_chemical_formula_weight         1471.05
_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                 93.440(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4845(5)
_cell_length_b                   20.2873(12)
_cell_length_c                   33.9574(18)
_cell_measurement_reflns_used    2216
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      63.33
_cell_measurement_theta_min      2.54
_cell_volume                     6522.1(6)
_computing_cell_refinement       SAINTPLUS
_computing_data_collection       SMART
_computing_data_reduction        SAINTPLUS
_computing_molecular_graphics    PLATON
_computing_publication_material  PLATON
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.683
_diffrn_measured_fraction_theta_max 0.683
_diffrn_measurement_device_type  'Bruker Smart 6000 CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_sigmaI/netI    0.2597
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12903
_diffrn_reflns_theta_full        63.33
_diffrn_reflns_theta_max         63.33
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    3.184
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.68587
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS in SaintPlus'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00171(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         7257
_refine_ls_number_restraints     1243
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.2825
_refine_ls_R_factor_gt           0.1027
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2330
_refine_ls_wR_factor_ref         0.3428
_reflns_number_gt                2216
_reflns_number_total             7257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205233d.txt
_cod_data_source_block           cs239
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7114047