Ca(ii), Yb(ii) and Tm(iii) complexes with tri- and tetra-anions of 1,2-bis[(2,6-diisopropylphenyl)imino]acenaphthene.
Fedushkin, Igor L.; Lukina, Daria A.; Skatova, Alexandra A.; Lukoyanov, Anton N.; Cherkasov, Anton V.; Chemical communications (Cambridge, England) 54 (2018) 12950–12953; doi:10.1039/c8cc08108e

data_7122541
_publ_section_title
;
 Ca(ii), Yb(ii) and Tm(iii) complexes with tri- and tetra-anions of
 1,2-bis[(2,6-diisopropylphenyl)imino]acenaphthene.
;
_journal_issue                   92
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12950
_journal_page_last               12953
_journal_paper_doi               10.1039/c8cc08108e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C104 H144 Ca2 N4 Na4 O8, 2(C4 H8 O)'
_chemical_formula_sum            'C112 H160 Ca2 N4 Na4 O10'
_chemical_formula_weight         1894.55
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-08-02 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                79.7990(10)
_cell_angle_beta                 85.2460(10)
_cell_angle_gamma                69.1460(10)
_cell_formula_units_Z            1
_cell_length_a                   13.0748(9)
_cell_length_b                   13.2572(9)
_cell_length_c                   15.9107(10)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.88
_cell_measurement_theta_min      2.74
_cell_volume                     2535.9(3)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXT-2017/1
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35764
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.367
_diffrn_reflns_theta_min         2.468
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         15181
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0741P)^2^+1.3580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11861
_reflns_number_total             15181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08108e2.cif
_cod_data_source_block           cabiannathf
_cod_depositor_comments
'Adding full bibliography for 7122540--7122542.cif.'
_cod_database_code               7122541
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              89326
_shelx_hkl_checksum              37871