Interaction of the trinuclear copper(I) pyrazolate with alkynes and carbon-carbon triple bond activation
Titov, Aleksei; Larionov, Vladimir A.; Smol’yakov, Alexander F.; Godovikova, Maria I.; Titova, Ekaterina M.; Maleev, Victor I.; Shubina, Elena; Chemical Communications  (2018) –; doi:10.1039/C8CC08592G

data_7122534
_publ_section_title
;
 Interaction of the trinuclear copper(I) pyrazolate with alkynes and
 carbon-carbon triple bond activation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08592G
_journal_year                    2018
_chemical_formula_moiety         'C36 H32 Cu3 F24 N8'
_chemical_formula_sum            'C36 H32 Cu3 F24 N8'
_chemical_formula_weight         1223.31
_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   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc20t5kl
_audit_creation_date             2018-10-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-03 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                107.62(3)
_cell_angle_beta                 100.88(2)
_cell_angle_gamma                95.18(2)
_cell_formula_units_Z            1
_cell_length_a                   8.550(9)
_cell_length_b                   10.660(12)
_cell_length_c                   13.468(14)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.691
_cell_measurement_theta_min      2.466
_cell_volume                     1135(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15153
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.571
_diffrn_reflns_theta_min         1.629
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0668 before and 0.0281 after correction. The Ratio of minimum to maximum transmission is 0.7654. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       plate
_exptl_crystal_F_000             607
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0382P)^2^+0.2851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6032
_reflns_number_total             6937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08592g2.cif
_cod_data_source_block           a_CCDC1
_cod_database_code               7122534
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.739
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b), C17(H17a,H17b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7)
2.c Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c)
;
_shelx_res_checksum              34867
_olex2_submission_special_instructions 'No special instructions were received'