Crystal structure of (OC‐6‐13)‐aqua‐tris (3‐bromopyridine‐κ1 N)‐bis(trifluoroacetato‐κ1 O)cadmium(II) C19H14Br3CdF6N3O5
Zhang, Lan; Wang, Lu; Ding, Wu-Xiu; Wang, Qiang; Chen, Meng-Juan; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 565–567; doi:10.1515/ncrs-2020-0631

data_8104768
_publ_section_title
;
 Crystal structure of (OC&#x2010;6&#x2010;13)&#x2010;aqua&#x2010;tris
 (3&#x2010;bromopyridine&#x2010;\k1
 N)&#x2010;bis(trifluoroacetato&#x2010;\k1 O)cadmium(II) C19H14Br3CdF6N3O5
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              565
_journal_page_last               567
_journal_paper_doi               10.1515/ncrs-2020-0631
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C19 H14 Br3 Cd F6 N3 O5'
_chemical_formula_sum            'C19 H14 Br3 Cd F6 N3 O5'
_chemical_formula_weight         830.46
_chemical_name_systematic
;
aqua-<i>\kO</i>-bis(<i>trans</i>-<i>\h</i>^1^-trifluoroacetato-<i>\kO</i>)-\
tris(3-bromopyridine-<i>\kN</i>)-cadmium(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   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                102.707(2)
_cell_angle_beta                 96.854(2)
_cell_angle_gamma                112.550(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2591(4)
_cell_length_b                   9.6573(5)
_cell_length_c                   16.9256(9)
_cell_measurement_reflns_used    9548
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.35
_cell_volume                     1328.20(12)
_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    'ShelXL (Sheldrick, 2015) [2]'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.448
_diffrn_reflns_theta_min         2.386
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.411
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0789 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.3514. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5452
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+2.0316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4422
_reflns_number_total             5452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0631_suppl.cif
_cod_data_source_block           mo_0114_2_0m
_cod_database_code               8104768
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(F6A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(F5A) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 F4, F4A, F5, F5A, F6, F6A, C4, C4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(C4A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4)=FVAR(1)
5.a Rotating group:
 O5(H5A,H5B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19)
;