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_7054850
_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         'C15 H3 Cu3 F18 N6, 2(C5 H4)'
_chemical_formula_sum            'C25 H11 Cu3 F18 N6'
_chemical_formula_weight         928.02
_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             2015-05-10
_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                109.803(2)
_cell_angle_beta                 117.447(2)
_cell_angle_gamma                95.807(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7936(11)
_cell_length_b                   12.4534(11)
_cell_length_c                   12.7263(11)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.30
_cell_measurement_theta_min      3.14
_cell_volume                     1484.7(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  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.984
_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  0.0134
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16256
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  0.8377
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0359 before and 0.0292 after correction.
The Ratio of minimum to maximum transmission is 0.7122.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.505
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6379
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0292P)^2^+1.1218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6098
_reflns_number_total             6379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01002k2.cif
_cod_data_source_block           rad194_0m_a_final
_cod_depositor_comments
'Adding full bibliography for 7054848--7054850.cif.'
_cod_database_code               7054850
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.393
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C9-F7 = C9-F8 = C9-F9 = C9A-F7A = C9A-F8A = C9A-F9A
 1.335 with sigma of 0.005
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.01
 F7A-F8A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.01
 C9-C6 \\sim C9A-C6
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F8A) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F7) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(C9) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C9) = Uanis(C9A)
4. Others
 Sof(C9A)=Sof(F8A)=Sof(F7A)=Sof(F9A)=1-FVAR(1)
 Sof(C9)=Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21),
 C22(H22), C23(H23), C24(H24)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'