Structural isomers of iron(III) N-methyl diethanolaminate as sol-gel precursors for iron-based oxide nanomaterials
Mishra, Shashank; Jeanneau, Erwann; Rolland, Marc; Daniele, Stephane; RSC Adv.  (2015) –; doi:10.1039/C5RA24627J

data_7223595
_publ_section_title
;
 Structural isomers of iron(III) N-methyl diethanolaminate as sol-gel
 precursors for iron-based oxide nanomaterials
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA24627J
_journal_year                    2015
_chemical_formula_moiety         'C30 H66 Fe4 N6 O12, 6(C H Cl3)'
_chemical_formula_sum            'C36 H72 Cl18 Fe4 N6 O12'
_chemical_formula_weight         1642.54
_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
_audit_creation_date             08-12-11
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2015-11-18 deposited with the CCDC.
2015-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                87.8178(10)
_cell_angle_beta                 80.2066(11)
_cell_angle_gamma                76.4053(11)
_cell_formula_units_Z            2
_cell_length_a                   11.38590(20)
_cell_length_b                   13.76370(29)
_cell_length_c                   22.75380(40)
_cell_measurement_reflns_used    15664
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.730
_cell_volume                     3415.38(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30710
_diffrn_reflns_theta_full        27.443
_diffrn_reflns_theta_max         28.003
_diffrn_reflns_theta_min         1.522
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.589
_exptl_absorpt_correction_T_max  0.8807
_exptl_absorpt_correction_T_min  0.8723
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.09
_refine_diff_density_min         -1.11
_refine_ls_extinction_coef       290(60)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1532
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9657
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.006426
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.38 1.03 1.02 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0959
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0837
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                10735
_reflns_number_total             16296
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0978
_oxford_refine_ls_scale          0.1339(3)
_oxford_reflns_number_all        16243
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'import in P -1'
_cod_data_source_file            c5ra24627j2.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        3415.379(114)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7223595