Tris(1-cyclopropyl-6-methyl-2-(<i>N</i>-methylaminocarbonyl)-4-oxo-1,4-dihydropyridin-4-olato)iron(III) dimethylformamide sesquisolvate dihydrate
Tam, Tim F.; Leung-Toung, Regis; Wang, Yingsheng; Spino, Michael; Lough, Alan J.; Acta Crystallographica Section E 61 (2005) m2601–m2603; doi:10.1107/S1600536805036251

data_2207520
_publ_section_title
;Tris(1-cyclopropyl-6-methyl-2-(<i>N</i>-methylaminocarbonyl)-4-oxo-1,4-dihydropyridin-4-olato)iron(III)
 dimethylformamide sesquisolvate dihydrate
;
_journal_coeditor_code           DN6272
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2601
_journal_page_last               m2603
_journal_paper_doi               10.1107/S1600536805036251
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe (C11 H13 N2 O3)3], 1.5C3 H7 N O, 2H2 O'
_chemical_formula_moiety         'C33 H39 Fe N6 O9, 1.5C3 H7 N O, 2H2 O'
_chemical_formula_sum            'C37.5 H53.5 Fe N7.5 O12.5'
_chemical_formula_weight         865.23
_chemical_name_systematic
;
Tris(1-cyclopropyl-6-methyl-2-N-methylaminocarbonyl-4-oxo-1,4-dihydropyridin-
4-olato)iron(III) dimethylformamide sesquisolvate dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                116.811(3)
_cell_angle_beta                 108.353(3)
_cell_angle_gamma                95.164(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9319(8)
_cell_length_b                   14.3968(9)
_cell_length_c                   15.3024(9)
_cell_measurement_reflns_used    20782
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.6
_cell_volume                     2141.6(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2003)'
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20782
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.463
_refine_diff_density_min         -0.492
_refine_ls_extinction_coef       0.0061(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0906P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                6632
_reflns_number_total             9756
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6272.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2141.6(2)
_cod_original_formula_sum        'C37.50 H53.50 Fe N7.50 O12.50'
_cod_database_code               2207520
_cod_database_fobs_code          2207520