Generation and transformation of a hemi-iminal-based metal-organic Fe(II) structure obtained via subcomponent self-assembly in water
Markiewicz, Grzegorz; Piechocki, Miłosz; Walczak, Anna; Połomska, Ewa; Harrowfield, Jack; Stefankiewicz, Artur Ryszard; Dalton Trans.  (2017) –; doi:10.1039/C7DT03182C

data_7044444
_publ_section_title
;
 Generation and transformation of a hemi-iminal-based metal-organic Fe(II)
 structure obtained via subcomponent self-assembly in water
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03182C
_journal_year                    2017
_chemical_formula_moiety         'C24 H16 Fe N6 O4, Cl O4'
_chemical_formula_sum            'C24 H16 Cl Fe N6 O8'
_chemical_formula_weight         607.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-05-22 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                107.694(2)
_cell_angle_beta                 105.087(2)
_cell_angle_gamma                99.040(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9536(2)
_cell_length_b                   11.9966(3)
_cell_length_c                   13.8709(3)
_cell_measurement_reflns_used    12971
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5460
_cell_measurement_theta_min      3.8690
_cell_volume                     1324.54(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00 -35.00   1.00    7.50    --  -20.49-178.00-120.00   80
  2  \w    -20.00  35.00   1.00    7.50    --  -20.49 -99.00   0.00   55
  3  \w    -96.00  17.00   1.00    7.50    --  -20.49 -57.00 150.00  113
  4  \w   -102.00  35.00   1.00    7.50    --  -20.49 -38.00   0.00  137
  5  \w    -96.00  17.00   1.00    7.50    --  -20.49 -57.00 -90.00  113
  6  \w    -54.00  60.00   1.00    7.50    --   21.74 -57.00 150.00  114
  7  \w    -54.00  60.00   1.00    7.50    --   21.74 -57.00 -90.00  114
  8  \w    -63.00  65.00   1.00    7.50    --   21.74 -77.00  60.00  128
  9  \w    -20.00  35.00   1.00    7.50    --  -20.49 -99.00-180.00   55
 10  \w    -58.00  56.00   1.00    7.50    --  -20.49  57.00  30.00  114
 11  \w    -58.00  56.00   1.00    7.50    --  -20.49  57.00-180.00  114
 12  \w    -96.00  17.00   1.00    7.50    --  -20.49 -57.00  90.00  113
 13  \w    -29.00  26.00   1.00    7.50    --   21.74  93.00-156.00   55
 14  \w     35.00 116.00   1.00    7.50    --   21.74 178.00 -30.00   81
 15  \w    -69.00 113.00   1.00    7.50    --   21.74   0.00-150.00  182
 16  \w    -69.00 113.00   1.00    7.50    --   21.74   0.00-120.00  182
 17  \w    -69.00 113.00   1.00    7.50    --   21.74   0.00 -90.00  182
 18  \w    -69.00 113.00   1.00    7.50    --   21.74   0.00 -60.00  182
 19  \w    -69.00 113.00   1.00    7.50    --   21.74   0.00 -30.00  182
 20  \w    -69.00 113.00   1.00    7.50    --   21.74   0.00-180.00  182
 21  \w    -69.00  89.00   1.00    7.50    --   21.74   0.00   0.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0546991000
_diffrn_orient_matrix_UB_12      0.0508247000
_diffrn_orient_matrix_UB_13      0.0433393000
_diffrn_orient_matrix_UB_21      -0.0252433000
_diffrn_orient_matrix_UB_22      0.0386617000
_diffrn_orient_matrix_UB_23      -0.0271715000
_diffrn_orient_matrix_UB_31      -0.0598148000
_diffrn_orient_matrix_UB_32      0.0067566000
_diffrn_orient_matrix_UB_33      0.0247040000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41842
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         4.103
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.4064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3636
_reflns_number_total             4442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03182c2.cif
_cod_data_source_block           2
_cod_database_code               7044444
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C24H16ClFeN6O8
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00F(H00F), C00I(H00I), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00W(H00W), C00Z(H00Z), C011(H011), C013(H013)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.899
_publcif_funding_html
;
;