Planar copper and nickel triangles with a guanidine-derived ligand
Matsumoto, Takuto; Sato, Yamato; Shiga, Takuya; Oshio, Hiroki; Inorganic Chemistry Frontiers 2 (2015) 725–; doi:10.1039/C5QI00085H

data_4348926
_publ_section_title
;
 Planar copper and nickel triangles with a guanidine-derived ligand
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              725
_journal_paper_doi               10.1039/C5QI00085H
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C33 H36 N15 Ni3 O6', 'B4 F16', 'C H4 O'
_chemical_formula_sum            'C34 H47 B4 F16 N15 Ni3 O7'
_chemical_formula_weight         1301.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                77.6660(10)
_cell_angle_beta                 83.379(2)
_cell_angle_gamma                83.524(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0521(8)
_cell_length_b                   11.4299(9)
_cell_length_c                   22.6136(18)
_cell_measurement_reflns_used    3126
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.3255
_cell_volume                     2510.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14336
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.035
_diffrn_reflns_theta_min         0.926
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  0.8865
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.975
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         9666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0861
_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^)+(0.1083P)^2^+12.2786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7159
_reflns_number_total             9666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00085h2.cif
_cod_data_source_block           '[Ni3]'
_cod_database_code               4348926
_shelx_estimated_absorpt_t_min   0.708
_shelx_estimated_absorpt_t_max   0.886
_shelxl_version_number           2013-4
_shelx_res_checksum              45626
_shelx_hkl_checksum              64455