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_7225187
_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         'C32 H24 Cu2 O10 S2'
_chemical_formula_sum            'C32 H24 Cu2 O10 S2'
_chemical_formula_weight         759.71
_chemical_name_systematic
di(chrysazinato)-bis(dimethylsulfoxide)-di-copper(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-08-18
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.90242(16)
_cell_length_b                   19.4909(4)
_cell_length_c                   18.5266(4)
_cell_measurement_reflns_used    7029
_cell_measurement_temperature    119.95(10)
_cell_measurement_theta_max      67.7770
_cell_measurement_theta_min      2.2630
_cell_volume                     2853.56(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_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
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0591
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.8954
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0148906000
_diffrn_orient_matrix_UB_12      0.0026522000
_diffrn_orient_matrix_UB_13      -0.0828709000
_diffrn_orient_matrix_UB_21      0.1152213000
_diffrn_orient_matrix_UB_22      -0.0637528000
_diffrn_orient_matrix_UB_23      0.0015480000
_diffrn_orient_matrix_UB_31      -0.1564135000
_diffrn_orient_matrix_UB_32      -0.0467131000
_diffrn_orient_matrix_UB_33      -0.0067340000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12638
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.846
_diffrn_reflns_theta_min         2.267
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.758
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.2214
_exptl_crystal_size_mid          0.1789
_exptl_crystal_size_min          0.0371
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 1859 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         4714
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0629P)^2^+1.6956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.817
_reflns_Friedel_fraction_max     0.813
_reflns_number_gt                4499
_reflns_number_total             4714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00792e2.cif
_cod_data_source_block           CuChrys-3
_cod_depositor_comments
'Adding full bibliography for 7225182--7225192.cif.'
_cod_database_code               7225187
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Cu2 C32 H24 O10 S2'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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,H,H,H) groups
2. Restrained distances
 S1B-O9 \\sim S1A-O9
 with sigma of 0.02
 S1B-C30 \\sim S1B-C29 \\sim S1A-C30 \\sim S1A-C29
 with sigma of 0.02
 S2B-O10 \\sim S2A-O10
 with sigma of 0.02
 S2B-C32 \\sim S2A-C32 \\sim S2A-C31 \\sim S2B-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S1B) = Uanis(S1A)
Uanis(S2B) = Uanis(S2A)
4. Others
 Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(S1B)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(S1A)=FVAR(1)
 Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(S2B)=1-FVAR(2)
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(S2A)=FVAR(2)
5.a Me refined with riding coordinates:
 C29(H29A,H29B,H29C), C29(H29D,H29E,H29F), C30(H30A,H30B,H30C), C30(H30D,H30E,
 H30F), C31(H31A,H31B,H31C), C31(H31D,H31E,H31F), C32(H32A,H32B,H32C), C32(H32D,
 H32E,H32F)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18),
 C26(H26), C27(H27), C28(H28)
;
_shelx_res_checksum              3556