Crystal structure of catena-poly[tetrakis(μ2-trifluoroacetato-κ2 O:O′)(μ2-2,5-dimethylpyrazine-κ2 N,N′)dicopper(II)], C7H4CuF6NO4
Zhang, Lan; Ren, Yong; Wang, Qiang; Ding, Wu-Xiu; Fei, Wen-Bo; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 875–877; doi:10.1515/ncrs-2020-0073

data_8105316
_publ_section_title
;
 Crystal structure of catena-poly[tetrakis(\m2-trifluoroacetato-\k2
 O:O&#x2032;)(\m2-2,5-dimethylpyrazine-\k2 N,N&#x2032;)dicopper(II)],
 C7H4CuF6NO4
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              875
_journal_page_last               877
_journal_paper_doi               10.1515/ncrs-2020-0073
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C7 H4 Cu F6 N O4'
_chemical_formula_sum            'C7 H4 Cu F6 N O4'
_chemical_formula_weight         343.65
_chemical_name_systematic
;
catena-poly[bis(\m2-\h1:\h1-trifluoroacetate-\k2 O:O')-
hemi(\m2-2,5-dimethylpyrazine-\k2 N,N')-copper(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                75.042(3)
_cell_angle_beta                 68.601(2)
_cell_angle_gamma                89.809(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5122(5)
_cell_length_b                   8.5458(6)
_cell_length_c                   8.8674(6)
_cell_measurement_reflns_used    7257
_cell_measurement_temperature    152.41
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.48
_cell_volume                     577.26(7)
_computing_cell_refinement       'SAINT (Bruker, 2016) [1]'
_computing_data_collection       'SAINT (Bruker, 2016) [1]'
_computing_data_reduction        'SAINT (Bruker, 2016) [1]'
_computing_molecular_graphics    'Diamond 4.0 [3]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [4]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [2]'
_computing_structure_solution    'ShelXT (Sheldrick, 2015) [2]'
_diffrn_ambient_temperature      152.41
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12313
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.442
_diffrn_reflns_theta_min         2.480
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int)
 was 0.0851 before and 0.0548 after correction. The Ratio of minimum to 
maximum transmission is 0.7768. The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_description       block
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2373
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0297P)^2^+0.3368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2162
_reflns_number_total             2373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0073_suppl.cif
_cod_data_source_block           mo_1223_1_0m
_cod_database_code               8105316
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.811
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2A) \\sim
Ueq, Uanis(F1A) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 F1, F2, F3, F2A, F1A, F3A, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F2A)=Sof(F1A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7)
5.b Idealised Me refined as rotating group:
 C6(H6B,H6A,H6C)
;