Acetylene and terminal alkyne complexes of copper(i) supported by fluorinated pyrazolates: syntheses, structures, and transformations.
Parasar, Devaborniny; Ponduru, Tharun T.; Noonikara-Poyil, Anurag; Jayaratna, Naleen B.; Dias, H. V. Rasika; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15782–15794; doi:10.1039/c9dt03350e

data_7701042
_publ_section_title
;
 Acetylene and terminal alkyne complexes of copper(i) supported by
 fluorinated pyrazolates: syntheses, structures, and transformations.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15782
_journal_page_last               15794
_journal_paper_doi               10.1039/c9dt03350e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C22 H20 Cu2 F12 N4'
_chemical_formula_sum            'C22 H20 Cu2 F12 N4'
_chemical_formula_weight         695.50
_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
_audit_creation_date             2017-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-06-18 deposited with the CCDC.    2019-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                97.7580(10)
_cell_angle_beta                 90.3530(10)
_cell_angle_gamma                107.1170(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4602(3)
_cell_length_b                   9.2660(4)
_cell_length_c                   17.3777(7)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      3.03
_cell_volume                     1288.50(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Bruker D8 Quest with a Photon 100 CMOS detector'
_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  0.0196
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17811
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.414
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.757
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0499 before and 0.0366 after correction. The Ratio of minimum to maximum transmission is 0.8953. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_description       plates
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0308P)^2^+0.8429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6796
_reflns_number_total             7741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03350e2.cif
_cod_data_source_block           rad517_0m_a
_cod_depositor_comments
'Adding full bibliography for 7701037--7701042.cif.'
_cod_database_code               7701042
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.678
_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:
 C15(H15A,H15B), C18(H18A,H18B), C16(H16A,H16B), C17(H17A,H17B), C21(H21A,
 H21B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C2(H2)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              47300
_olex2_submission_special_instructions 'No special instructions were received'