Self-assembly synthesis, structure, topology, and magnetic properties of a mononuclear Fe(iii)-violurate derivative: a combined experimental and theoretical study.
Banik, Rupak; Roy, Subhadip; Dlháň, Ľubor; Titiš, Ján; Boča, Roman; Kirillov, Alexander M.; Martin, Adam D.; Bauza, Antonio; Frontera, Antonio; Rodríguez-Diéguez, Antonio; Salas, Juan M.; Das, Subrata; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16166–16172; doi:10.1039/c6dt03139k

data_7040682
_publ_section_title
;
 Self-assembly synthesis, structure, topology, and magnetic properties of
 a mononuclear Fe(iii)-violurate derivative: a combined experimental and
 theoretical study.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16166
_journal_page_last               16172
_journal_paper_doi               10.1039/c6dt03139k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 H6 Fe N9 O12, C5 H5 N, 4(H2 O)'
_chemical_formula_sum            'C17 H19 Fe N10 O16'
_chemical_formula_weight         675.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-30
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-09-03 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.062(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4941(13)
_cell_length_b                   14.2216(15)
_cell_length_c                   14.0514(14)
_cell_measurement_reflns_used    8822
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.970
_cell_measurement_theta_min      2.614
_cell_volume                     2516.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26605
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.970
_diffrn_reflns_theta_min         2.614
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7226
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+1.1529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5616
_reflns_number_total             7226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03139k2.cif
_cod_data_source_block           r47_0m
_cod_depositor_comments          'Adding full bibliography for 7040682.cif.'
_cod_database_code               7040682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{N1S, C1S}
{C6S, N6S}
3. Uiso/Uaniso restraints and constraints
Uanis(N1S) = Uanis(C1S)
Uanis(C6S) = Uanis(N6S)
4. Rigid body (RIGU) restrains
 N1S, C3S, C4S, C2S, C5S, C6S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: H5S(0.5) H5SA(0.5) C6S(0.5) H6S(0.5) N1S(0.5) H2S(0.5) H2SA(0.5)
 C1S(0.5) H1S(0.5) N6S(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB)
6.b Free rotating group:
 O2W(H2WA,H2WB), O4W(H4WA,H4WB)
6.c Aromatic/amide H refined with riding coordinates:
 N12(H12), N13(H13), N22(H22), N23(H23), N32(H32), N33(H33), C3S(H3S),
 C4S(H4S), C5S(H5S), C5S(H5SA), C6S(H6S), C2S(H2S), C2S(H2SA), C1S(H1S)
;
_shelx_res_checksum              73048
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'