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_7225184
_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
'2(C68 H52 Co4 N4 O20), 2.35(C3 H7 N O), 0.5(O)'
_chemical_formula_sum            'C143.05 H120.45 Co8 N10.35 O42.85'
_chemical_formula_weight         3141.48
_chemical_name_systematic
'di[tetra(chrysazinato)-tetra(N,N-dimethylformamide)-tetra-cobalt(II)] di(N,N-dimethylformamide) solvate hemihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-05
_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                90.9201(10)
_cell_angle_beta                 104.1390(16)
_cell_angle_gamma                90.2340(13)
_cell_formula_units_Z            2
_cell_length_a                   15.6278(16)
_cell_length_b                   15.6996(15)
_cell_length_c                   29.048(3)
_cell_measurement_reflns_used    19366
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     6909.9(12)
_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
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
scan:
    Number of images: 330
               Slice: -95.0000 - 70.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 18.0000
                 Phi: -180.0000
                 XTD: 50.0076
              2theta: -20.0488
scan:
    Number of images: 180
               Slice: -69.0000 - 21.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -90.0000
                 XTD: 50.0076
              2theta: -20.0488
scan:
    Number of images: 204
               Slice: -32.0000 - 70.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: -150.0000
                 XTD: 50.0076
              2theta: -20.0488
scan:
    Number of images: 178
               Slice: -69.0000 - 20.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 90.0000
                 XTD: 50.0076
              2theta: -20.0488
scan:
    Number of images: 52
               Slice: -34.0000 - -8.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 54.0000
                 Phi: 60.0000
                 XTD: 50.0076
              2theta: -20.0488
scan:
    Number of images: 330
               Slice: -95.0000 - 70.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 18.0000
                 Phi: 30.0000
                 XTD: 50.0076
              2theta: -20.0488
scan:
    Number of images: 182
               Slice: -70.0000 - 21.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 120.0000
                 XTD: 50.0076
              2theta: -20.0488
scan:
    Number of images: 204
               Slice: -32.0000 - 70.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: 60.0000
                 XTD: 50.0076
              2theta: -20.0488
scan:
    Number of images: 22
               Slice: -69.0000 - -58.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -60.0000
                 XTD: 50.0076
              2theta: -20.0488

;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support MiTeGen
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.055508
_diffrn_orient_matrix_UB_12      0.013734
_diffrn_orient_matrix_UB_13      -0.032938
_diffrn_orient_matrix_UB_21      0.003197
_diffrn_orient_matrix_UB_22      -0.060149
_diffrn_orient_matrix_UB_23      -0.020746
_diffrn_orient_matrix_UB_31      -0.011235
_diffrn_orient_matrix_UB_32      0.009851
_diffrn_orient_matrix_UB_33      -0.032210
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            119113
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.602
_diffrn_reflns_theta_min         2.256
_diffrn_reflns_transf_matrix_11  0.055508
_diffrn_reflns_transf_matrix_12  0.013734
_diffrn_reflns_transf_matrix_13  -0.032938
_diffrn_reflns_transf_matrix_21  0.003197
_diffrn_reflns_transf_matrix_22  -0.060149
_diffrn_reflns_transf_matrix_23  -0.020746
_diffrn_reflns_transf_matrix_31  -0.011235
_diffrn_reflns_transf_matrix_32  0.009851
_diffrn_reflns_transf_matrix_33  -0.032210
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3220
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         1.698
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2078
_refine_ls_number_reflns         31716
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+16.1538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27773
_reflns_number_total             31716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00792e2.cif
_cod_data_source_block           CoChrys-3
_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        6909.8(12)
_cod_database_code               7225184
_shelxl_version_number           2014/6
_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. Restrained distances
 O40-C162 = O40-C161
 1.21 with sigma of 0.01
 C172-N10 = C171-N10
 1.44 with sigma of 0.01
 C171-O42
 2.78 with sigma of 0.01
 C170-N10
 1.3 with sigma of 0.01
 O42-C170
 1.21 with sigma of 0.01
 C162-N8B = C161-N8A
 1.3 with sigma of 0.01
 O41-C167
 1.21 with sigma of 0.01
 C168-O41
 2.78 with sigma of 0.01
 C167-N9
 1.3 with sigma of 0.01
 C168-N9 = C169-N9
 1.44 with sigma of 0.01
 N8A-C163 = N8A-C165 = N8B-C166 = N8B-C164
 1.44 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N4 \\sim C67 \\sim C68: within 1.7A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C137) \\sim Ueq, Uanis(C136) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.005
Uanis(C175) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C174) \\sim Ueq, Uanis(C173)
\\sim Ueq, Uanis(O43) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.05
Uanis(C170) \\sim Ueq, Uanis(C171) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(N10)
\\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.005
Uanis(C167) \\sim Ueq, Uanis(C168) \\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(N9)
\\sim Ueq, Uanis(O41) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(C108) = Uanis(C109)
Uanis(C110) = Uanis(C111)
Uanis(C99) = Uanis(C117)
Uanis(C118) = Uanis(C119)
Uanis(C106) = Uanis(C107)
Uanis(C96) = Uanis(C97)
Uanis(C98) = Uanis(C99)
Uanis(C145) = Uanis(C144)
Uanis(O36A) = Uanis(O36B)
Uanis(C125) = Uanis(C4)
Uanis(C137) = Uanis(C136)
Uanis(C145) = Uanis(C144)
Uanis(C127) = Uanis(C126)
Uanis(C135) = Uanis(C134)
Uanis(C139) = Uanis(C138)
Uanis(C147) = Uanis(C146)
Uanis(C96) = Uanis(C97)
Uanis(C106) = Uanis(C107)
Uanis(C108) = Uanis(C109)
Uanis(C110) = Uanis(C111)
Uanis(C116) = Uanis(C117)
Uanis(C118) = Uanis(C119)
Uanis(C120) = Uanis(C121)
Uanis(C122) = Uanis(C123)
Uanis(C112) = Uanis(C113)
Uanis(C114) = Uanis(C115)
Uanis(C104) = Uanis(C105)
Uanis(C102) = Uanis(C103)
Uanis(C100) = Uanis(C101)
Uanis(C98) = Uanis(C99)
Uanis(C96) = Uanis(C97)
Uanis(C144) = Uanis(C145)
Uanis(C146) = Uanis(C147)
Uanis(C148) = Uanis(C149)
Uanis(C150) = Uanis(C151)
Uanis(C140) = Uanis(C141)
Uanis(C138) = Uanis(C139)
Uanis(C142) = Uanis(C143)
Uanis(O36A) = Uanis(O36B)
Uanis(C136) = Uanis(C137)
Uanis(C134) = Uanis(C135)
Uanis(C132) = Uanis(C133)
Uanis(C4) = Uanis(C125)
Uanis(C126) = Uanis(C127)
Uanis(C128) = Uanis(C129)
Uanis(C130) = Uanis(C131)
Uanis(C132) = Uanis(C133)
4. Others
 Sof(C125)=Sof(C127)=Sof(H127)=Sof(C129)=Sof(H129)=Sof(C131)=Sof(H131)=
 Sof(C133)=Sof(C135)=Sof(C137)=Sof(C139)=Sof(C141)=Sof(C143)=Sof(C145)=
 Sof(C147)=Sof(H147)=Sof(C149)=Sof(H149)=Sof(C151)=Sof(H151)=Sof(O36B)=1-FVAR(1)
 Sof(C4)=Sof(C126)=Sof(H126)=Sof(C128)=Sof(H128)=Sof(C130)=Sof(H130)=Sof(C132)=
 Sof(C134)=Sof(C136)=Sof(C138)=Sof(C140)=Sof(C142)=Sof(C144)=Sof(C146)=
 Sof(H146)=Sof(C148)=Sof(H148)=Sof(C150)=Sof(H150)=Sof(O36A)=FVAR(1)
 Fixed Sof: O41(0.5) O42(0.5) N9(0.5) N10(0.5) C96(0.5) C97(0.5) C98(0.5)
 H98(0.5) C99(0.5) H99(0.5) C100(0.5) H100(0.5) C101(0.5) H101(0.5) C102(0.5)
 H102(0.5) C103(0.5) H103(0.5) C104(0.5) C105(0.5) C106(0.5) C107(0.5)
 C108(0.5) C109(0.5) C110(0.5) C111(0.5) C112(0.5) C113(0.5) C114(0.5)
 C115(0.5) C116(0.5) C117(0.5) C118(0.5) H118(0.5) C119(0.5) H119(0.5)
 C120(0.5) H120(0.5) C121(0.5) H121(0.5) C122(0.5) H122(0.5) C123(0.5)
 H123(0.5) C161(0.5) H161(0.5) C162(0.5) H162(0.5) C163(0.5) H16D(0.5)
 H16E(0.5) H16F(0.5) C164(0.5) H16G(0.5) H16H(0.5) H16I(0.5) C165(0.5)
 H16J(0.5) H16K(0.5) H16L(0.5) C166(0.5) H16M(0.5) H16N(0.5) H16O(0.5)
 C167(0.5) H167(0.5) C168(0.5) H16P(0.5) H16Q(0.5) H16R(0.5) C169(0.5)
 H16S(0.5) H16T(0.5) H16U(0.5) C170(0.5) H170(0.5) C171(0.5) H17A(0.5)
 H17B(0.5) H17C(0.5) C172(0.5) H17D(0.5) H17E(0.5) H17F(0.5) O32A(0.5) N8A(0.5)
 C40A(0.5) H40A(0.5) C41A(0.5) H41A(0.5) C42A(0.5) H42A(0.5) C54A(0.5)
 H54A(0.5) C55A(0.5) H55A(0.5) C56A(0.5) H56A(0.5) O32B(0.5) N8B(0.5) C40B(0.5)
 H40B(0.5) C41B(0.5) H41B(0.5) C42B(0.5) H42B(0.5) C54B(0.5) H54B(0.5)
 C55B(0.5) H55B(0.5) C56B(0.5) H56B(0.5) O1W(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C10(H10), C13(H13), C14(H14), C18(H18), C26(H26), C27(H27),
 C32(H32), C44(H44), C45(H45), C46(H46), C57(H57), C60(H60), C66(H66), C70(H70),
  C71(H71), C72(H72), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85),
 C86(H86), C93(H93), C94(H94), C95(H95), C98(H98), C99(H99), C100(H100),
 C101(H101), C102(H102), C103(H103), C118(H118), C119(H119), C120(H120),
 C121(H121), C122(H122), C123(H123), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C146(H146), C147(H147), C148(H148),
 C149(H149), C150(H150), C151(H151), C152(H152), C155(H155), C158(H158),
 C161(H161), C162(H162), C167(H167), C170(H170), C173(H173), C1A(H1A),
 C40A(H40A), C41A(H41A), C42A(H42A), C54A(H54A), C55A(H55A), C56A(H56A),
 C40B(H40B), C41B(H41B), C42B(H42B), C54B(H54B), C55B(H55B), C56B(H56B),
 C1G(H1G), C1N(H1N), C1O(H1O), C1Q(H1Q), C1T(H1T), C1V(H1V)
5.b Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C153(H15A,H15B,H15C), C154(H15D,H15E,H15F), C156(H15G,H15H,H15I),
 C157(H15J,H15K,H15L), C159(H15M,H15N,H15O), C160(H16A,H16B,H16C), C163(H16D,
 H16E,H16F), C164(H16G,H16H,H16I), C165(H16J,H16K,H16L), C166(H16M,H16N,H16O),
 C168(H16P,H16Q,H16R), C169(H16S,H16T,H16U), C171(H17A,H17B,H17C), C172(H17D,
 H17E,H17F), C174(H17G,H17H,H17I), C175(H17J,H17K,H17L)
;
_shelx_res_checksum              66526