Iron molybdenum nitrilotriacetate and iminodiacetate ‒ spectroscopy, structural characterization and CO2 adsorption
Wang, Si-Yuan; Dong, Xin; Chen, Jun-Fei; Zhou, Zhao-Hui; New Journal of Chemistry 42 (2018) 18526–; doi:10.1039/C8NJ03475C

data_7057865
_publ_section_title
;
 Iron molybdenum nitrilotriacetate and iminodiacetate -- spectroscopy,
 structural characterization and CO2 adsorption
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18526
_journal_paper_doi               10.1039/C8NJ03475C
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C32 H40 Fe8 Mo2 N8 O40'
_chemical_formula_sum            'C32 H40 Fe8 Mo2 N8 O40'
_chemical_formula_weight         1815.40
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-25 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   9.7754(2)
_cell_length_b                   9.7754(2)
_cell_length_c                   13.7948(4)
_cell_measurement_reflns_used    2263
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.5970
_cell_measurement_theta_min      2.5480
_cell_volume                     1318.21(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_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    -41.00  48.00   1.00   10.00    --  -22.85  57.00 120.00   89
  2  \w    -21.00   8.00   1.00   10.00    --   24.10  99.00-106.00   29
  3  \w     35.00  60.00   1.00   10.00    --   24.10  57.00-180.00   25
  4  \w    -92.00   1.00   1.00   10.00    --  -22.85 -57.00-120.00   93
  5  \w     77.00 106.00   1.00   10.00    --   24.10-178.00-150.00   29
  6  \w     78.00 104.00   1.00   10.00    --   24.10-178.00 120.00   26
  7  \w    -71.00 -42.00   1.00   10.00    --  -22.85-178.00  90.00   29
  8  \w    -96.00  -3.00   1.00   10.00    --  -22.85 -38.00 -30.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0651613000
_diffrn_orient_matrix_UB_12      -0.0256973000
_diffrn_orient_matrix_UB_13      0.0134543000
_diffrn_orient_matrix_UB_21      -0.0103397000
_diffrn_orient_matrix_UB_22      -0.0236687000
_diffrn_orient_matrix_UB_23      -0.0480160000
_diffrn_orient_matrix_UB_31      0.0302644000
_diffrn_orient_matrix_UB_32      -0.0635908000
_diffrn_orient_matrix_UB_33      0.0124758000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5335
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.904
_diffrn_reflns_theta_min         2.554
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.821
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.218
_refine_ls_abs_structure_details
;
 Flack x determined using 340 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.20(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.335
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0600
_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^)+36.7463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.675
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                938
_reflns_number_total             950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03475c2.cif
_cod_data_source_block           exp_17632
_cod_depositor_comments
'Adding full bibliography for 7057864--7057867.cif.'
_cod_original_cell_volume        1318.21(7)
_cod_database_code               7057865
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.613
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_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 1.087
_oxdiff_exptl_absorpt_empirical_full_min 0.945