Structural diversity of copper(I) ethylene complexes with 2,4-bis(2-pyridyl)pyrimidine directed by anions
Maekawa, Masahiko; Hayashi, Terumasa; Sugimoto, Kunihisa; Okubo, Takashi; Kuroda-Sowa, T.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02618C

data_7714010
_publ_section_title
;
 Structural diversity of copper(I) ethylene complexes with
 2,4-bis(2-pyridyl)pyrimidine directed by anions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02618C
_journal_year                    2023
_chemical_formula_moiety         'C30 H24 Cu3 N8, C32 H28 Cu3 N8, 6(B F4)'
_chemical_formula_sum            'C62 H52 B6 Cu6 F24 N16'
_chemical_formula_weight         1923.29
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-06-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-04 deposited with the CCDC.	2023-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.594(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7929(6)
_cell_length_b                   11.3730(2)
_cell_length_c                   29.0946(7)
_cell_measurement_reflns_used    21077
_cell_measurement_temperature    97.15
_cell_measurement_theta_max      31.73
_cell_measurement_theta_min      2.76
_cell_volume                     7105.3(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      97.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Rigaku XtaLAB PRO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            50700
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.411
_diffrn_reflns_theta_min         2.768
_exptl_absorpt_coefficient_mu    1.881
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       plate
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.683
_refine_diff_density_min         -1.635
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         10738
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+19.7521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9477
_reflns_number_total             10738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02618c2.cif
_cod_data_source_block           4-cu-bpprd-u-c2h4-bf4
_cod_database_code               7714010
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C31-H31a = C31-H31b
 0.99 with sigma of 0.02
 C30-H30b = C30-H30a
 0.99 with sigma of 0.02
 C29-H29b = C29-H29a
 0.99 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(H29b) = Uiso(H29a)
Uiso(H31a) = Uiso(H31b) = Uiso(H30b) = Uiso(H30a)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27)
;
_shelx_res_checksum              64801
_olex2_submission_special_instructions 'No special instructions were received'