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_7701041
_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         'C26 H14 Cu2 F12 N4'
_chemical_formula_sum            'C26 H14 Cu2 F12 N4'
_chemical_formula_weight         737.49
_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             2019-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-18 deposited with the CCDC.    2019-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                71.399(3)
_cell_angle_beta                 71.758(2)
_cell_angle_gamma                79.715(2)
_cell_formula_units_Z            4
_cell_length_a                   12.9771(15)
_cell_length_b                   13.6360(15)
_cell_length_c                   17.588(3)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.95
_cell_volume                     2790.7(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      175.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35889
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.129
_diffrn_reflns_theta_min         2.950
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0496 before and 0.0405 after correction. The Ratio of minimum to maximum transmission is 0.8889. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.597
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         14970
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0771P)^2^+2.7681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11883
_reflns_number_total             14970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03350e2.cif
_cod_data_source_block           rad230_0m_a
_cod_depositor_comments
'Adding full bibliography for 7701037--7701042.cif.'
_cod_original_cell_volume        2790.7(6)
_cod_database_code               7701041
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.737
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F24A-C36 \\sim F22-C36 \\sim F22A-C36 \\sim F23-C36 \\sim F23A-C36 \\sim
F24-C36
 with sigma of 0.02
 F13-C30 \\sim F13A-C30 \\sim F14A-C30 \\sim F14-C30 \\sim F15-C30 \\sim
F15A-C30
 with sigma of 0.02
 F13-F14 \\sim F13-F15 \\sim F14-F15 \\sim F13A-F14A \\sim F13A-F15A \\sim
F14A-F15A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F24A) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F22A) \\sim Ueq, Uanis(F23)
\\sim Ueq, Uanis(F23A) \\sim Ueq, Uanis(F24) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(F15A) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14A)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
4. Others
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C33(H33),
  C37(H37), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
;
_shelx_res_checksum              85677
_olex2_submission_special_instructions 'No special instructions were received'