Isolable arene sandwiched copper(i) pyrazolates
Jayaratna, Naleen B.; Hettiarachchi, Champika V.; Yousufuddin, Muhammed; Rasika Dias, H. V.; New J. Chem. 39 (2015) 5092–; doi:10.1039/C5NJ01002K

data_7054848
_publ_section_title
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 Isolable arene sandwiched copper(i) pyrazolates
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              5092
_journal_paper_doi               10.1039/C5NJ01002K
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         '2(C15 H3 Cu3 F18 N6), 2(C3 H3)'
_chemical_formula_sum            'C36 H12 Cu6 F36 N12'
_chemical_formula_weight         1677.82
_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
_audit_creation_date             2015-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-10 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                88.897(7)
_cell_angle_beta                 84.185(7)
_cell_angle_gamma                87.425(7)
_cell_formula_units_Z            2
_cell_length_a                   9.560(4)
_cell_length_b                   12.620(5)
_cell_length_c                   21.550(8)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.72
_cell_measurement_theta_min      2.96
_cell_volume                     2583.7(18)
_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  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.03
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28553
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.962
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.600
_exptl_absorpt_correction_T_max  0.8789
_exptl_absorpt_correction_T_min  0.5315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0516 before and 0.0418 after correction.
The Ratio of minimum to maximum transmission is 0.6047.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.157
_exptl_crystal_description       platy
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         11227
_refine_ls_number_restraints     1122
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0510P)^2^+3.0821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9039
_reflns_number_total             11227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01002k2.cif
_cod_data_source_block           rad200_0m_a_final
_cod_depositor_comments
'Adding full bibliography for 7054848--7054850.cif.'
_cod_original_cell_volume        2583.8(17)
_cod_database_code               7054848
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.433
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 F1, F2, F3, F4, F5, F6, F7, F8, F9, F10, F11, F12, F13, F14, F15, F16, F17,
 F18, F19, F20, F21, F22, F23, F24, F25, F26, F27, F28, F29, F30, F31, F32, F33,
  F34, F35, F36, F7A, F9A, F8A, F34A, F35A, F36A, C1, C2, C3, C4, C5, C6, C7,
 C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23,
 C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17
\\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim F25
\\sim F26 \\sim F27 \\sim F28 \\sim F29 \\sim F30 \\sim F31 \\sim F32 \\sim F33
\\sim F34 \\sim F35 \\sim F36 \\sim F7A \\sim F9A \\sim F8A \\sim F34A \\sim
F35A \\sim F36A \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15
\\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23
\\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31
\\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq,
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11)
\\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq,
Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18)
\\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq,
Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F25)
\\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F28) \\sim Ueq,
Uanis(F29) \\sim Ueq, Uanis(F30) \\sim Ueq, Uanis(F31) \\sim Ueq, Uanis(F32)
\\sim Ueq, Uanis(F33) \\sim Ueq, Uanis(F34) \\sim Ueq, Uanis(F35) \\sim Ueq,
Uanis(F36) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F8A)
\\sim Ueq, Uanis(F34A) \\sim Ueq, Uanis(F35A) \\sim Ueq, Uanis(F36A) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(F7)=Sof(F9)=Sof(F8A)=1-FVAR(1)
 Sof(F8)=Sof(F7A)=Sof(F9A)=FVAR(1)
 Sof(F34A)=Sof(F35A)=Sof(F36A)=1-FVAR(2)
 Sof(F34)=Sof(F35)=Sof(F36)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C17(H17), C22(H22), C27(H27), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'