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_7225192
_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         'C40 H36 N8 Ni2 O20'
_chemical_formula_sum            'C40 H36 N8 Ni2 O20'
_chemical_formula_weight         1066.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.517(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5780(7)
_cell_length_b                   11.0933(8)
_cell_length_c                   20.1508(14)
_cell_measurement_reflns_used    13941
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     2111.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
scan:

    Number of images: 108

               Slice: -35.0000 - 73.0000

         Image width: 1.0000

            Exp time: 90.0000

       Rotation axis: Omega

               Omega: 0.0000

               Kappa: 72.0000

                 Phi: 150.0000

                 XTD: 45.1653

              2theta: -16.9738

scan:

    Number of images: 91

               Slice: -69.0000 - 22.0000

         Image width: 1.0000

            Exp time: 90.0000

       Rotation axis: Omega

               Omega: 0.0000

               Kappa: -72.0000

                 Phi: 30.0000

                 XTD: 45.1653

              2theta: -16.9738

scan:

    Number of images: 90

               Slice: -68.0000 - 22.0000

         Image width: 1.0000

            Exp time: 90.0000

       Rotation axis: Omega

               Omega: 0.0000

               Kappa: -72.0000

                 Phi: -150.0000

                 XTD: 45.1653

              2theta: -16.9738

scan:

    Number of images: 64

               Slice: -56.0000 - 8.0000

         Image width: 1.0000

            Exp time: 90.0000

       Rotation axis: Omega

               Omega: 0.0000

               Kappa: 0.0000

                 Phi: -180.0000

                 XTD: 45.1653

              2theta: -16.9738

scan:

    Number of images: 20

               Slice: -2.0000 - 18.0000

         Image width: 1.0000

            Exp time: 90.0000

       Rotation axis: Omega

               Omega: 0.0000

               Kappa: -36.0000

                 Phi: -150.0000

                 XTD: 45.1653

              2theta: -16.9738

scan:

    Number of images: 95

               Slice: -63.0000 - 32.0000

         Image width: 1.0000

            Exp time: 90.0000

       Rotation axis: Omega

               Omega: 0.0000

               Kappa: 18.0000

                 Phi: -90.0000

                 XTD: 45.1653

              2theta: -16.9738
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.117
_diffrn_reflns_av_unetI/netI     0.063
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15440
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         2.752
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4722
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0486P)^2^+6.9532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2879
_reflns_number_total             4722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00792e2.cif
_cod_data_source_block           NiNOChrys-1
_cod_depositor_comments
'Adding full bibliography for 7225182--7225192.cif.'
_cod_database_code               7225192
_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
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of
0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C12(H12), C13(H13), C15(H15), C18(H18)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'