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_7225185
_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         'C28 H12 Cu2 O8'
_chemical_formula_sum            'C28 H12 Cu2 O8'
_chemical_formula_weight         603.46
_chemical_name_systematic        di(chrysazinato)-di-copper(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.380(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5308(3)
_cell_length_b                   7.7288(2)
_cell_length_c                   19.6854(4)
_cell_measurement_reflns_used    5267
_cell_measurement_temperature    120
_cell_measurement_theta_max      71.1060
_cell_measurement_theta_min      6.1540
_cell_volume                     2031.11(8)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9454
_diffrn_measurement_details
;
  1 omega   37.00   63.00   1.0000   10.2300
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 26

  2 omega  -25.00   29.00   1.0000   10.2300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -60.0000 54

  3 omega  -16.00   17.00   1.0000   10.2300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 33

  4 omega   77.00  124.00   1.0000   32.4000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  -90.0000 47

  5 omega    2.00   58.00   1.0000   32.4000
omega____ theta____ kappa____ phi______ frames
    -       54.7500 -125.0000  -30.0000 56

  6 omega -111.00  -13.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000 -180.0000 98

  7 omega -124.00  -44.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -63.0000   30.0000 80

  8 omega   38.00   67.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000    0.0000 29

  9 omega   43.00  113.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000 -150.0000 70

 10 omega   43.00   70.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   30.0000 27

 11 omega   39.00   66.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   90.0000 27

 12 omega   41.00   66.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000    0.0000 25

 13 omega   46.00   72.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   90.0000 26

 14 omega  110.00  136.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 26

 15 omega   73.00  140.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  -30.0000 67

 16 omega   41.00   67.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   90.0000 26

 17 omega   44.00   71.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 27

 18 omega   39.00   65.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -30.0000 26

 19 omega   41.00   66.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -90.0000 25

 20 omega   41.00   67.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  -30.0000 26

 21 omega  138.00  171.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000 -120.0000 33

 22 omega   42.00   70.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   60.0000 28

 23 omega   74.00  176.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000  150.0000 102

 24 omega   38.00   68.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  150.0000 30

 25 omega   88.00  113.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000   90.0000 25

 26 omega   39.00   64.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   30.0000 25

 27 omega  118.00  154.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000   86.0000  134.0000 36

 28 omega   40.00   67.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 27

 29 omega   80.00  113.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000 -120.0000 33

 30 omega   82.00  107.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   30.0000 25

 31 omega   42.00   79.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -150.0000 37

 32 omega   39.00   64.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0637731000
_diffrn_orient_matrix_UB_12      0.0445412000
_diffrn_orient_matrix_UB_13      0.0699813000
_diffrn_orient_matrix_UB_21      -0.0572158000
_diffrn_orient_matrix_UB_22      0.1720077000
_diffrn_orient_matrix_UB_23      0.0014754000
_diffrn_orient_matrix_UB_31      -0.0772843000
_diffrn_orient_matrix_UB_32      -0.0903004000
_diffrn_orient_matrix_UB_33      0.0373474000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.200
_diffrn_reflns_theta_min         3.311
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.131
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.762
_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_primary    black
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.1319
_exptl_crystal_size_mid          0.1101
_exptl_crystal_size_min          0.0245
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+2.1374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3468
_reflns_number_total             3926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00792e2.cif
_cod_data_source_block           CuChrys-1
_cod_depositor_comments
'Adding full bibliography for 7225182--7225192.cif.'
_cod_original_cell_volume        2031.10(9)
_cod_database_code               7225185
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Cu2 C28 O8 H8'
_reflns_odcompleteness_completeness 94.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C28(H28), C27(H27), C21(H21), C23(H23), C15(H15), C9(H9), C8(H8),
 C7(H7), C1(H1), C22(H22), C14(H14)
;
_shelx_res_checksum              69321