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_7057866
_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         '0.5(C48 H92 Cr4 Mo4 N8 Na12 O84), 4(H2 O)'
_chemical_formula_sum            'C24 H54 Cr2 Mo2 N4 Na6 O46'
_chemical_formula_weight         1568.50
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-09
_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                 107.693(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.5265(7)
_cell_length_b                   11.0330(6)
_cell_length_c                   16.5498(10)
_cell_measurement_reflns_used    3961
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.0860
_cell_measurement_theta_min      2.7480
_cell_volume                     2700.9(3)
_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 0.872
_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    -42.00  41.00   1.00   14.00    --  -23.01 -19.00  30.00   83
  2  \w    -95.00  15.00   1.00   14.00    --  -23.01   0.00 150.00  110
  3  \w     61.00  88.00   1.00   14.00    --   24.26 178.00 150.00   27
  4  \w     65.00 104.00   1.00   14.00    --   24.26 178.00 120.00   39
;
_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      0.0153371000
_diffrn_orient_matrix_UB_12      -0.0108360000
_diffrn_orient_matrix_UB_13      -0.0355901000
_diffrn_orient_matrix_UB_21      0.0420630000
_diffrn_orient_matrix_UB_22      -0.0205967000
_diffrn_orient_matrix_UB_23      0.0272859000
_diffrn_orient_matrix_UB_31      -0.0172347000
_diffrn_orient_matrix_UB_32      -0.0599349000
_diffrn_orient_matrix_UB_33      -0.0029559000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13034
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.846
_diffrn_reflns_theta_min         2.253
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90368
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_description       plate
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.145
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6786
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+17.5632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5940
_reflns_number_total             6786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03475c2.cif
_cod_data_source_block           exp_17485
_cod_depositor_comments
'Adding full bibliography for 7057864--7057867.cif.'
_cod_database_code               7057866
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.686
_reflns_odcompleteness_completeness 99.89
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H3WA-O3W = H3WB-O3W = H4WA-O4W = H4WB-O4W = H1WA-O1W = H1WB-O1W
 0.85 with sigma of 0.01
 H3WA-H3WB = H4WA-H4WB = H1WA-H1WB
 1.388 with sigma of 0.001
3. Others
 Fixed Sof: Na4(0.5) O6WB(0.5) O6WA(0.5)
4.a Free rotating group:
 O7W(H7WA,H7WB), O8W(H8WA,H8WB)
4.b Rotating group:
 O5W(H5WA,H5WB), O2W(H2WA,H2WB)
4.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C11(H11A,H11B), C1(H1A,H1B), C7(H7A,H7B), C9(H9A,H9B), C3(H3A,H3B)
;
_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 1.134
_oxdiff_exptl_absorpt_empirical_full_min 0.888