#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:27:12 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230496 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/78/7057865.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7057865
loop_
_publ_author_name
'Wang, Si-Yuan'
'Dong, Xin'
'Chen, Jun-Fei'
'Zhou, Zhao-Hui'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  48.00   1.00   10.00    --  -22.85  57.00 120.00   89
  2  ω    -21.00   8.00   1.00   10.00    --   24.10  99.00-106.00   29
  3  ω     35.00  60.00   1.00   10.00    --   24.10  57.00-180.00   25
  4  ω    -92.00   1.00   1.00   10.00    --  -22.85 -57.00-120.00   93
  5  ω     77.00 106.00   1.00   10.00    --   24.10-178.00-150.00   29
  6  ω     78.00 104.00   1.00   10.00    --   24.10-178.00 120.00   26
  7  ω    -71.00 -42.00   1.00   10.00    --  -22.85-178.00  90.00   29
  8  ω    -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       'ω 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/[σ²(Fo²)+36.7463P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_iucr_refine_instructions_details
;

    exp_17632.res created by SHELXL-2014/7

TITL exp_17632_a.res in I-42m
REM Old TITL exp_17632 in I4/mmm
REM SHELXT solution in I-42m
REM R1 0.082, Rweak 0.057, Alpha 0.015, Orientation as input
REM Flack x = -0.079 ( 0.032 ) from Parsons' quotients
REM Formula found by SHELXT: C24 N16 Mo Fe4
CELL 0.71073 9.7754 9.7754 13.7948 90 90 90
ZERR 1 0.0002 0.0002 0.0004 0 0 0
LATT -2
SYMM -X,-Y,+Z
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM -Y,-X,+Z
SYMM +Y,+X,+Z
SFAC C H Fe Mo N O
UNIT 32 40 8 2 8 40
 
L.S. 10
PLAN  20
SIZE 0.2 0.1 0.1
TEMP -100.15
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\exp_17632.hkl">
REM </olex2.extras>
 
WGHT    0.000000   36.746304
FVAR       0.41003
MO1   4    0.000000    0.000000    0.500000    10.12500    0.00683    0.00683 =
         0.00767    0.00000    0.00000    0.00000
FE1   3    0.196785    0.196785    0.688669    10.50000    0.01310    0.01310 =
         0.00985    0.00034    0.00034   -0.00200
O2    6    0.510231    0.276431    0.748380    11.00000    0.00878    0.08069 =
         0.01291   -0.00814   -0.00097   -0.00360
O1    6    0.388653    0.182959    0.630818    11.00000    0.01641    0.03977 =
         0.02742   -0.01387   -0.00325   -0.00365
N1    5    0.749584    0.250416    0.659690    10.50000    0.01201    0.01201 =
         0.01804   -0.00466    0.00466    0.00033
AFIX  13
H1    2    0.821879    0.178123    0.662119    10.50000   -1.20000
AFIX   0
O3    6    0.105055    0.105055    0.574160    10.50000    0.02119    0.02119 =
         0.01716   -0.00062   -0.00062   -0.00747
C2    1    0.499867    0.220600    0.667759    11.00000    0.01264    0.02388 =
         0.01687    0.00493   -0.00309   -0.00189
C1    1    0.630842    0.191264    0.611338    11.00000    0.01670    0.02832 =
         0.01890   -0.01687    0.00207    0.00084
AFIX  23
H1A   2    0.643337    0.091126    0.605294    11.00000   -1.20000
H1B   2    0.622902    0.229905    0.545240    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  exp_17632_a.res in I-42m
REM R1 =  0.0600 for     938 Fo > 4sig(Fo)  and  0.0607 for all     950 data
REM     57 parameters refined using      0 restraints
 
END  
     
WGHT      0.0000     36.7468 

REM Highest difference peak  0.821,  deepest hole -1.557,  1-sigma level  0.218
Q1    1   0.5000  0.5000  0.5803  10.25000  0.05    0.82
Q2    1   0.2949  0.2949  0.6006  10.50000  0.05    0.80
Q3    1   0.5307  0.4693  0.5379  10.50000  0.05    0.80
Q4    1   0.0000  0.0000  0.4097  10.25000  0.05    0.79
Q5    1   0.0000  0.0000  0.6425  10.25000  0.05    0.77
Q6    1   0.5696  0.1964  0.6839  11.00000  0.05    0.75
Q7    1   0.7873  0.2127  0.7241  10.50000  0.05    0.74
Q8    1   0.1057  0.0180  0.5525  11.00000  0.05    0.74
Q9    1   0.7262  0.0971  0.6304  11.00000  0.05    0.73
Q10   1   0.0000  0.1925  0.5000  10.50000  0.05    0.72
Q11   1   0.1439  0.1185  0.6319  11.00000  0.05    0.71
Q12   1   0.2038  0.2509  0.6125  11.00000  0.05    0.71
Q13   1   0.5000  0.5000  0.6750  10.25000  0.05    0.70
Q14   1   0.5934  0.4066  0.6409  10.50000  0.05    0.69
Q15   1   0.6032  0.3968  0.5418  10.50000  0.05    0.68
Q16   1   0.7746  0.2254  0.5020  10.50000  0.05    0.67
Q17   1   0.7721  0.0000  0.6118  11.00000  0.05    0.65
Q18   1   0.5563  0.4437  0.6182  10.50000  0.05    0.64
Q19   1   0.5000  0.4122  0.5000  10.50000  0.05    0.63
Q20   1   0.8994  0.1006  0.6715  10.50000  0.05    0.63

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0600 for 938 Fo > 4sig(Fo) and 0.0607 for all 5335 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.82, deepest hole -1.56
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0607
  REM R1_gt = 0.0600
  REM wR_ref = 0.1384
  REM GOOF = 1.335
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 5335
  REM Reflections_gt = 938
  REM Parameters = n/a
  REM Hole = -1.56
  REM Peak = 0.82
  REM Flack = -0.20(3)

  
;
_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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mo1 Mo 0.0000 0.0000 0.5000 0.0071(5) Uani 1 8 d S T P
Fe1 Fe 0.19679(15) 0.19679(15) 0.68867(14) 0.0120(5) Uani 1 2 d S T P
O2 O 0.5102(10) 0.2764(11) 0.7484(6) 0.034(2) Uani 1 1 d . . .
O1 O 0.3887(8) 0.1830(11) 0.6308(6) 0.028(2) Uani 1 1 d . . .
N1 N 0.7496(10) 0.2504(10) 0.6597(9) 0.014(2) Uani 1 2 d S T P
H1 H 0.8219 0.1781 0.6621 0.017 Uiso 1 2 calc RS T P
O3 O 0.1051(8) 0.1051(8) 0.5742(7) 0.020(2) Uani 1 2 d S T P
C2 C 0.4999(13) 0.2206(10) 0.6678(7) 0.018(2) Uani 1 1 d . . .
C1 C 0.6308(11) 0.1913(14) 0.6113(8) 0.021(2) Uani 1 1 d . . .
H1A H 0.6433 0.0911 0.6053 0.026 Uiso 1 1 calc R . .
H1B H 0.6229 0.2299 0.5452 0.026 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0068(6) 0.0068(6) 0.0077(10) 0.000 0.000 0.000
Fe1 0.0131(6) 0.0131(6) 0.0098(9) 0.0003(6) 0.0003(6) -0.0020(8)
O2 0.009(4) 0.081(7) 0.013(3) -0.008(4) -0.001(3) -0.004(5)
O1 0.016(4) 0.040(6) 0.027(4) -0.014(4) -0.003(3) -0.004(4)
N1 0.012(3) 0.012(3) 0.018(6) -0.005(3) 0.005(3) 0.000(4)
O3 0.021(3) 0.021(3) 0.017(6) -0.001(3) -0.001(3) -0.007(5)
C2 0.013(4) 0.024(5) 0.017(4) 0.005(4) -0.003(5) -0.002(5)
C1 0.017(5) 0.028(6) 0.019(5) -0.017(5) 0.002(4) 0.001(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 Mo1 O3 109.7(7) 4_556 3_556
O3 Mo1 O3 109.7(7) 2 .
O3 Mo1 O3 109.4(3) 3_556 .
O3 Mo1 O3 109.4(3) 3_556 2
O3 Mo1 O3 109.4(3) 4_556 2
O3 Mo1 O3 109.4(3) 4_556 .
O2 Fe1 O2 92.8(6) 14_456 12_546
O2 Fe1 O1 89.4(4) 12_546 .
O2 Fe1 O1 89.4(4) 14_456 8
O2 Fe1 O1 175.7(4) 14_456 .
O2 Fe1 O1 175.7(4) 12_546 8
O2 Fe1 N1 77.1(3) 14_456 12_546
O2 Fe1 N1 77.1(3) 12_546 12_546
O1 Fe1 O1 88.2(6) 8 .
O1 Fe1 N1 99.8(4) . 12_546
O1 Fe1 N1 99.8(4) 8 12_546
O3 Fe1 O2 89.6(3) . 12_546
O3 Fe1 O2 89.6(3) . 14_456
O3 Fe1 O1 94.2(3) . 8
O3 Fe1 O1 94.2(3) . .
O3 Fe1 N1 160.5(5) . 12_546
C2 O2 Fe1 120.7(9) . 11_556
C2 O1 Fe1 128.1(7) . .
C1 N1 Fe1 109.8(6) 7_665 11_556
C1 N1 Fe1 109.8(6) . 11_556
C1 N1 C1 115.0(14) . 7_665
Mo1 O3 Fe1 163.9(6) . .
O2 C2 O1 124.2(12) . .
O2 C2 C1 118.1(11) . .
O1 C2 C1 117.7(8) . .
N1 C1 C2 111.1(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 1.776(11) 4_556
Mo1 O3 1.776(11) .
Mo1 O3 1.776(11) 3_556
Mo1 O3 1.776(11) 2
Fe1 O2 2.037(10) 12_546
Fe1 O2 2.037(10) 14_456
Fe1 O1 2.043(9) 8
Fe1 O1 2.043(9) .
Fe1 N1 2.216(12) 12_546
Fe1 O3 2.026(11) .
O2 Fe1 2.037(10) 11_556
O2 C2 1.243(12) .
O1 C2 1.256(14) .
N1 Fe1 2.216(12) 11_556
N1 C1 1.458(13) .
N1 C1 1.458(13) 7_665
C2 C1 1.526(15) .
