Preparation and Crystal Structure of Tetrakis(μ-2,4,5-trimethoxybenzoato-κ<i>O</i>:κ<i>O</i>′)bis[(methanol)copper(II)]-<i>N,N</i>-dimethylformamide (1/2) in Relation to Adsorption Property for N<sub>2</sub>
MIKURIYA, Masahiro; YAMAKAWA, Chihiro; TANABE, Kensuke; NUKITA, Raigo; YOSHIOKA, Daisuke; MITSUHASHI, Ryoji; TANAKA, Hidekazu; HANDA, Makoto; TSUBOI, Motohiro; X-ray Structure Analysis Online 37 (2021) 35–37; doi:10.2116/xraystruct.37.35

data_1564542
_publ_section_title
;
 Preparation and Crystal Structure of
 Tetrakis(\m-2,4,5-trimethoxybenzoato-\k&lt;i&gt;O&lt;/i&gt;:\k&lt;i&gt;O&lt;/i&gt;&#x2032;)bis[(methanol)copper(II)]-&lt;i&gt;N,N&lt;/i&gt;-dimethylformamide
 (1/2) in Relation to Adsorption Property for N&lt;sub&gt;2&lt;/sub&gt;
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              35
_journal_page_last               37
_journal_paper_doi               10.2116/xraystruct.37.35
_journal_volume                  37
_journal_year                    2021
_chemical_formula_sum            'C48 H66 Cu2 N2 O24'
_chemical_formula_weight         1182.10
_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   mixed
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                65.354(2)
_cell_angle_beta                 65.025(2)
_cell_angle_gamma                72.661(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2532(13)
_cell_length_b                   11.6634(13)
_cell_length_c                   12.3118(14)
_cell_measurement_reflns_used    3769
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.59
_cell_volume                     1316.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8490
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.932
_diffrn_reflns_theta_min         1.938
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       platelet
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0442P)^2^+0.5773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5418
_reflns_number_total             6035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            37_35_1.txt
_cod_data_source_block           CuCY61m_0m
_cod_database_code               1564542
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.893
_shelx_res_checksum              95658
_shelx_hkl_checksum              42407