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_7225186
_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            'C29.33 H15.11 Cu2 N0.44 O8.44'
_chemical_formula_weight         635.77
_chemical_name_systematic
'di(chrysazinato)di-copper(II) N,N'-dimethylformamide solvate'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2015-11-22
_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                120
_cell_formula_units_Z            9
_cell_length_a                   40.04(3)
_cell_length_b                   40.04(3)
_cell_length_c                   3.674(3)
_cell_measurement_reflns_used    4306
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      1.7
_cell_volume                     5101(7)
_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_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
scan:
    Number of images: 175
               Slice: -60.0000 - 115.0000
         Image width: 1.0000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 59.8393
              2theta: 30.1018
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 0.0000
                 XTD: 59.8393
              2theta: 30.1018
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 120.0000
                 XTD: 59.8393
              2theta: 30.1018
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 240.0000
                 XTD: 59.8393
              2theta: 30.1018
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.028544
_diffrn_orient_matrix_UB_12      -0.003106
_diffrn_orient_matrix_UB_13      -0.002664
_diffrn_orient_matrix_UB_21      0.017754
_diffrn_orient_matrix_UB_22      0.019917
_diffrn_orient_matrix_UB_23      0.010936
_diffrn_orient_matrix_UB_31      0.007218
_diffrn_orient_matrix_UB_32      -0.135882
_diffrn_orient_matrix_UB_33      0.235753
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            16552
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.603
_diffrn_reflns_theta_min         1.708
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       needle
_exptl_crystal_F_000             2877
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.517
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0686P)^2^+23.2644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2481
_reflns_number_total             2587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00792e2.cif
_cod_data_source_block           CuChrys-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7225182--7225192.cif.
;
_cod_original_cell_volume        5101(9)
_cod_database_code               7225186
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.02) H3(0.021) H4(0.02) H8(0.024) H9(0.024) H10(0.021)
 Fixed X: H2(0.371301) H3(0.371901) H4(0.4278) H8(0.558801) H9(0.611301)
 H10(0.6104)
 Fixed Y: H2(0.3574) H3(0.3029) H4(0.3075) H8(0.3814) H9(0.4403) H10(0.4963)
 Fixed Z: H2(-0.148299) H3(0.0297) H4(0.2787) H8(0.721301) H9(0.910399)
 H10(0.8328)
;
_shelx_res_checksum              14919
_platon_squeeze_void_probe_radius 1.20