A Ni8metallacalix[4]arene and a Cu4molecular rhomboid: limiting the nuclearity of carboxysalen-like metal complexes
Fondo, Matilde; Doejo, Jesús; García-Deibe, Ana M.; Sanmartín-Matalobos, Jesús; Vicente, Ramón; CrystEngComm 18 (2016) 6673–; doi:10.1039/C6CE01384H

data_7225986
_publ_section_title
;
 A Ni8metallacalix[4]arene and a Cu4molecular rhomboid: limiting the
 nuclearity of carboxysalen-like metal complexes
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6673
_journal_paper_doi               10.1039/C6CE01384H
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C76 H88 N8 Ni8 O40, 7(C H4 O), 12(O H2)'
_chemical_formula_sum            'C83 H140 N8 Ni8 O59'
_chemical_formula_weight         2663.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-07-13 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   16.1124(4)
_cell_measurement_reflns_used    9133
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.66
_cell_measurement_theta_min      2.435
_cell_volume                     13882.4(5)
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_collection       'BRUKER APEX2'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-2008 (Burla, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1123
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            82208
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.387
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.8721
_exptl_absorpt_correction_T_min  0.7892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       prism
_exptl_crystal_F_000             5560
_exptl_crystal_size_max          0.230
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_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.978
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_refine_ls_extinction_coef       0.00075(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.1720
_refine_ls_R_factor_gt           0.0940
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2893
_refine_ls_wR_factor_ref         0.3578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3072
_reflns_number_total             6154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01384h1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7225986--7225987.cif.'
_cod_original_cell_volume        13882.4(7)
_cod_database_code               7225986
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.875
_shelxl_version_number           2013-4
_shelx_res_checksum              20715