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_7225182
_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         'C126 H114 Co12 N6 O54'
_chemical_formula_sum            'C144 H156 Co12 N12 O60'
_chemical_formula_weight         3721.96
_chemical_name_systematic
'dodeca(acetato)-hexa(chrysazinato)-hexa(N,N-dimethylformamide)-dodeca-cobalt(II) hexa(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   geom
_audit_creation_date             2016-03-17
_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            3
_cell_length_a                   28.6873(9)
_cell_length_b                   28.6873(9)
_cell_length_c                   15.9087(10)
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      24.6250
_cell_measurement_theta_min      2.0780
_cell_volume                     11338.2(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9028
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0228332000
_diffrn_orient_matrix_UB_12      0.0176141000
_diffrn_orient_matrix_UB_13      -0.0243408000
_diffrn_orient_matrix_UB_21      0.0161368000
_diffrn_orient_matrix_UB_22      -0.0072435000
_diffrn_orient_matrix_UB_23      0.0242296000
_diffrn_orient_matrix_UB_31      -0.0057589000
_diffrn_orient_matrix_UB_32      -0.0212763000
_diffrn_orient_matrix_UB_33      -0.0284412000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17691
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.166
_diffrn_reflns_theta_min         2.080
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_density_diffrn    1.635
_exptl_crystal_description       prism
_exptl_crystal_F_000             5724
_exptl_crystal_size_max          0.1896
_exptl_crystal_size_mid          0.1651
_exptl_crystal_size_min          0.1012
_platon_squeeze_details
;
;
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5582
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0619P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3063
_reflns_number_total             5582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00792e2.cif
_cod_data_source_block           CoChrys-1
_cod_depositor_comments
'Adding full bibliography for 7225182--7225192.cif.'
_cod_original_cell_volume        11338.2(10)
_cod_database_code               7225182
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Co12 C141 H149 N11 O59'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Uiso/Uaniso restraints and constraints
O1 \\sim C1: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.001
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C19(H19)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C)
;
_shelx_res_checksum              26230