#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:03:35 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224175 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/94/7049447.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7049447
loop_
_publ_author_name
'Parasar, Devaborniny'
'Jayaratna, Naleen B.'
'Muñoz-Castro, Alvaro'
'Conway, Allison E.'
'Mykhailiuk, Pavel K.'
'Dias, H. V. Rasika'
_publ_section_title
;
 Carbonyl complexes of copper(i) stabilized by bridging fluorinated
 pyrazolates and halide ions.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6358
_journal_page_last               6371
_journal_paper_doi               10.1039/c9dt00486f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C14 Cu2 F18 N4 O2'
_chemical_formula_sum            'C14 Cu2 F18 N4 O2'
_chemical_formula_weight         725.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-31 deposited with the CCDC.    2019-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.012(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.702(4)
_cell_length_b                   18.154(5)
_cell_length_c                   8.944(2)
_cell_measurement_reflns_used    5555
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      3.03
_cell_volume                     2183.8(10)
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker D8 Quest with a Photon 100 CMOS detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10473
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.173
_diffrn_reflns_theta_min         3.029
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_T_max  0.3352
_exptl_absorpt_correction_T_min  0.2918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0422 before and 0.0338 after correction. The Ratio of minimum to maximum transmission is 0.8705. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0266
_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/[σ²(Fo²)+(0.0293P)²+4.5403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2627
_reflns_number_total             3038
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00486f2.cif
_cod_data_source_block           rad152_0m_a
_cod_depositor_comments
'Adding full bibliography for 7049446--7049452.cif.'
_cod_database_code               7049447
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.608
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu Cu 0.19929(2) 0.59103(2) 0.30074(2) 0.01697(7) Uani 1 1 d . . .
F1 F 0.37106(10) 0.67987(7) 0.32476(17) 0.0355(3) Uani 1 1 d . . .
F2 F 0.52617(10) 0.65662(8) 0.33537(19) 0.0431(4) Uani 1 1 d . . .
F3 F 0.42826(14) 0.66750(7) 0.11850(17) 0.0473(4) Uani 1 1 d . . .
F4 F 0.64281(15) 0.500000 0.3550(2) 0.0606(8) Uani 1 2 d S T P
F5 F 0.59866(10) 0.44142(8) 0.14587(19) 0.0425(4) Uani 1 1 d . . .
F6 F 0.19810(11) 0.65378(8) 0.78277(16) 0.0397(3) Uani 1 1 d . . .
F7 F 0.17511(12) 0.68177(7) 0.54453(16) 0.0381(3) Uani 1 1 d . . .
F8 F 0.04976(10) 0.66681(7) 0.65422(16) 0.0343(3) Uani 1 1 d . . .
F9 F 0.18749(18) 0.500000 0.9629(2) 0.0521(6) Uani 1 2 d S T P
F10 F 0.05444(15) 0.44062(10) 0.88271(18) 0.0575(5) Uani 1 1 d . . .
O O 0.10448(17) 0.71357(11) 0.1092(2) 0.0545(5) Uani 1 1 d . . .
N1 N 0.32244(11) 0.53746(7) 0.27971(16) 0.0160(3) Uani 1 1 d . . .
N2 N 0.15692(11) 0.53762(8) 0.47218(17) 0.0167(3) Uani 1 1 d . . .
C1 C 0.41250(13) 0.56024(9) 0.26056(19) 0.0168(3) Uani 1 1 d . . .
C2 C 0.47305(19) 0.500000 0.2467(3) 0.0173(5) Uani 1 2 d S T P
C3 C 0.43455(16) 0.64121(11) 0.2586(2) 0.0261(4) Uani 1 1 d . . .
C4 C 0.5779(2) 0.500000 0.2233(3) 0.0247(5) Uani 1 2 d S T P
C5 C 0.13896(13) 0.56031(10) 0.6072(2) 0.0176(3) Uani 1 1 d . . .
C6 C 0.12635(19) 0.500000 0.6979(3) 0.0186(5) Uani 1 2 d S T P
C7 C 0.14026(15) 0.64090(11) 0.6469(2) 0.0238(4) Uani 1 1 d . . .
C8 C 0.1051(2) 0.500000 0.8552(3) 0.0268(6) Uani 1 2 d S T P
C9 C 0.13980(17) 0.66666(12) 0.1817(3) 0.0297(4) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Cu N2 102.25(6) . .
C9 Cu N1 127.13(8) . .
C9 Cu N2 130.53(8) . .
N1 N1 Cu 119.30(4) 6_565 .
C1 N1 Cu 132.76(12) . .
C1 N1 N1 107.93(9) . 6_565
N2 N2 Cu 119.13(4) 6_565 .
C5 N2 Cu 132.34(12) . .
C5 N2 N2 107.87(10) . 6_565
N1 C1 C2 110.32(16) . .
N1 C1 C3 119.65(16) . .
C2 C1 C3 130.03(17) . .
C1 C2 C1 103.5(2) . 6_565
C1 C2 C4 128.25(11) 6_565 .
C1 C2 C4 128.25(11) . .
F1 C3 F2 106.75(17) . .
F1 C3 C1 111.02(16) . .
F2 C3 C1 111.68(17) . .
F3 C3 F1 107.32(18) . .
F3 C3 F2 107.08(17) . .
F3 C3 C1 112.68(17) . .
F4 C4 C2 112.0(2) . .
F5 C4 F4 106.69(17) 6_565 .
F5 C4 F4 106.69(17) . .
F5 C4 F5 106.3(2) 6_565 .
F5 C4 C2 112.39(16) . .
F5 C4 C2 112.39(16) 6_565 .
N2 C5 C6 110.30(16) . .
N2 C5 C7 120.96(16) . .
C6 C5 C7 128.63(16) . .
C5 C6 C5 103.7(2) . 6_565
C5 C6 C8 128.17(11) . .
C5 C6 C8 128.17(11) 6_565 .
F6 C7 F8 106.70(16) . .
F6 C7 C5 111.24(17) . .
F7 C7 F6 107.35(17) . .
F7 C7 F8 107.09(17) . .
F7 C7 C5 111.60(15) . .
F8 C7 C5 112.56(16) . .
F9 C8 C6 112.9(2) . .
F10 C8 F9 105.37(18) . .
F10 C8 F9 105.37(18) 6_565 .
F10 C8 F10 108.3(3) 6_565 .
F10 C8 C6 112.20(16) . .
F10 C8 C6 112.20(16) 6_565 .
O C9 Cu 179.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N1 1.9873(15) .
Cu N2 1.9921(15) .
Cu C9 1.831(2) .
F1 C3 1.340(2) .
F2 C3 1.340(3) .
F3 C3 1.329(3) .
F4 C4 1.333(4) .
F5 C4 1.329(2) .
F6 C7 1.338(2) .
F7 C7 1.336(2) .
F8 C7 1.339(2) .
F9 C8 1.337(4) .
F10 C8 1.330(2) .
O C9 1.123(3) .
N1 N1 1.360(3) 6_565
N1 C1 1.343(2) .
N2 N2 1.366(3) 6_565
N2 C5 1.343(2) .
C1 C2 1.392(2) .
C1 C3 1.501(3) .
C2 C4 1.491(4) .
C5 C6 1.393(2) .
C5 C7 1.505(3) .
C6 C8 1.490(4) .
