Spontaneous ligand nitrosation and self-assembly into a pentacopper metallacrown complex.
Otsuki, Joe; Sekine, Tatsuki; Kida, Yuki; Shinozaki, Yoshinao; Kobayashi, Sayaka; Tamura, Takahiro; Sugawa, Kosuke; Yoshikawa, Isao; Houjou, Hirohiko; Yoshikawa, Hiroki; Tsukamoto, Arata; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2760–2764; doi:10.1039/c6dt04696g

data_7041986
_publ_section_title
;
 Spontaneous ligand nitrosation and self-assembly into a pentacopper
 metallacrown complex.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2760
_journal_page_last               2764
_journal_paper_doi               10.1039/c6dt04696g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
;
'(C20 H28 Cu4.78 N12 O12), 7.44(H2 O), 1.56(N O3)'
;
_chemical_formula_sum            'C20 H42.88 Cu4.78 N13.56 O24.12'
_chemical_formula_weight         1163.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-20 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.993(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.965(4)
_cell_length_b                   20.231(5)
_cell_length_c                   13.227(3)
_cell_measurement_reflns_used    5976
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.60
_cell_volume                     3961.3(17)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r3'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r3'
_computing_molecular_graphics
;
'ShelXle (Sheldrick, 2011) and OLEX2 (Dolomanov et al., 2009)'
;
_computing_publication_material
;
'SHELXL-2014/7 (Sheldrick, 2014) and local procedure'
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'VariMax DW with Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13421
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.366
_diffrn_reflns_theta_min         2.610
_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   REQAB(Rigaku,1998)
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       plate
_exptl_crystal_F_000             2349
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00052(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         3632
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0576P)^2^+5.0790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3069
_reflns_number_total             3632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04696g2.cif
_cod_data_source_block           dalton_9
_cod_depositor_comments          'Adding full bibliography for 7041986.cif.'
_cod_database_code               7041986
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.584
_shelx_estimated_absorpt_t_max   0.799
_shelx_res_checksum              3385