Synthesis and structural characterisation of the novel iron helicate [Fe2(μ-L)4(μ-Cl)2][FeCl4]2 and metalla-macrocycle [Fe2(μ-L)2(THF)4Cl2][FeCl4]2{L =N,N'-di(n-butylcarbamoyl)pyridine-2,6-dicarboxamide}
Hayley A. Burkill; Ramón Vilar; Andrew J. P. White; David J. Williams; J. Chem. Soc., Dalton Trans.  (2002) 837–839; doi:10.1039/b200191h

data_7011459
_publ_section_title
;
 Synthesis and structural characterisation of the novel iron helicate
 [Fe2(\m-L)4(\m-Cl)2][FeCl4]2 and metalla-macrocycle
 [Fe2(\m-L)2(THF)4Cl2][FeCl4]2{L
 =N,N'-di(n-butylcarbamoyl)pyridine-2,6-dicarboxamide}
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              837
_journal_page_last               839
_journal_paper_doi               10.1039/b200191h
_journal_year                    2002
_chemical_formula_sum            'C56 H94 Cl10 Fe4 N10 O13.5'
_chemical_formula_weight         1701.31
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.411(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1655(14)
_cell_length_b                   18.797(2)
_cell_length_c                   22.468(2)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.94
_cell_volume                     4192.9(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.1242
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7714
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        21.80
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.7935
_exptl_absorpt_correction_T_min  0.3965
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange/brown
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       'prismatic needles'
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0007(4)
_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_all   0.999
_refine_ls_goodness_of_fit_obs   1.171
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         5800
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.165
_refine_ls_R_factor_all          0.1923
_refine_ls_R_factor_obs          0.0742
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2342
_refine_ls_wR_factor_obs         0.1588
_reflns_number_observed          3037
_reflns_number_total             7278
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b200191h.txt
_cod_data_source_block           RV0118
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4192.9(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C56 H94 N10 O13.50 Cl10 Fe4'
_cod_database_code               7011459