Transition metal coordination complexes of chrysazin
Beldon, Patrick J.; Henke, Sebastian; Monserrat, Bartomeu; Tominaka, Satoshi; Stock, Norbert; Cheetham, Anthony K.; CrystEngComm 18 (2016) 5121–; doi:10.1039/C5CE00792E

data_7225188
_publ_section_title
;
 Transition metal coordination complexes of chrysazin
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              5121
_journal_paper_doi               10.1039/C5CE00792E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C34 H28 Fe N2 O10'
_chemical_formula_sum            'C34 H28 Fe N2 O10'
_chemical_formula_weight         680.43
_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             2016-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.448(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0131(4)
_cell_length_b                   8.4169(4)
_cell_length_c                   18.1414(8)
_cell_measurement_reflns_used    2527
_cell_measurement_temperature    269.95(10)
_cell_measurement_theta_max      67.4910
_cell_measurement_theta_min      4.7180
_cell_volume                     1503.59(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      269.95(10)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -25.00    2.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -      -26.1037  -99.0000  -60.0000 27

  2 omega  -96.00  -68.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -      -26.1037 -178.0000   60.0000 28

  3 omega  -13.00   27.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -      -26.1037  -99.0000  -30.0000 40

  4 omega   -8.00   43.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -       26.1037   57.0000  150.0000 51

  5 omega   47.00   93.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -       26.1037   57.0000  150.0000 46

  6 omega -154.00 -127.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      -67.8019  -94.0000   30.0000 27

  7 omega  -95.00  -47.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      -67.8019  -61.0000  -60.0000 48

  8 omega -143.00 -102.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      -67.8019  -61.0000  -60.0000 41

  9 omega   88.00  133.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019  111.0000  -60.0000 45

 10 omega   39.00  136.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019   61.0000  120.0000 97

 11 omega   13.00   81.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019  -94.0000 -120.0000 68

 12 omega  -19.00    7.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019  -94.0000 -120.0000 26

 13 omega  -16.00   50.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019  -30.0000 -150.0000 66

 14 omega   31.00   56.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   21.0000    0.0000 25

 15 omega  105.00  131.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000    0.0000 26

 16 omega   31.00   71.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -43.0000  150.0000 40

 17 omega   90.00  119.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000  -30.0000 29

 18 omega  110.00  178.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  104.0000 -180.0000 68

 19 omega   32.00   60.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -43.0000   30.0000 28

 20 omega   74.00  122.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000  -60.0000 48

 21 omega  123.00  150.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -21.0000   90.0000 27

 22 omega   30.00   73.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -43.0000   90.0000 43

 23 omega   36.00   75.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -43.0000 -150.0000 39

 24 omega  125.00  177.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -21.0000  150.0000 52

 25 omega   58.00  152.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000 -180.0000 94

 26 omega  126.00  167.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000  -30.0000 41

 27 omega  140.00  168.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -32.0000  -90.0000 28

 28 omega  151.00  178.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000    0.0000 27

 29 omega   52.00   78.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -104.0000  150.0000 26

 30 omega  121.00  154.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   21.0000    0.0000 33

 31 omega   48.00   73.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -65.0000 -150.0000 25

 32 omega  144.00  172.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -32.0000  120.0000 28

 33 omega  116.00  145.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -21.0000  -30.0000 29

 34 omega  133.00  174.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -32.0000   60.0000 41
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1300217000
_diffrn_orient_matrix_UB_12      0.0399622000
_diffrn_orient_matrix_UB_13      -0.0304284000
_diffrn_orient_matrix_UB_21      -0.0696005000
_diffrn_orient_matrix_UB_22      0.1488298000
_diffrn_orient_matrix_UB_23      -0.0387647000
_diffrn_orient_matrix_UB_31      0.0523363000
_diffrn_orient_matrix_UB_32      0.0985416000
_diffrn_orient_matrix_UB_33      0.0709530000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5822
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.438
_diffrn_reflns_theta_max         67.438
_diffrn_reflns_theta_min         4.719
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.584
_exptl_absorpt_correction_T_max  0.488
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.4481
_exptl_crystal_size_mid          0.2249
_exptl_crystal_size_min          0.1057
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0725P)^2^+0.1511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2349
_reflns_number_total             2679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00792e2.cif
_cod_data_source_block           FeChrys-1
_cod_depositor_comments
'Adding full bibliography for 7225182--7225192.cif.'
_cod_original_cell_volume        1503.60(12)
_cod_database_code               7225188
_chemical_oxdiff_formula         'Fe2 C34 N2 O10 H26'
_reflns_odcompleteness_completeness 93.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_shelxl_version_number     2014/7