Macrocyclic complexes of Pt(ii) and Rh(iii) with iso-tellurazole N-oxides.
Ho, Peter C.; Bui, Robert; Cevallos, Alberto; Sequeira, Shanel; Britten, James F.; Vargas-Baca, Ignacio; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4879–4886; doi:10.1039/c9dt00500e

data_7049314
_publ_section_title
;
 Macrocyclic complexes of Pt(ii) and Rh(iii) with iso-tellurazole
 N-oxides.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4879
_journal_page_last               4886
_journal_paper_doi               10.1039/c9dt00500e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C10 H9 Cl0.5 N O Rh0.25 Te, B0.25 F'
_chemical_formula_sum            'C10 H9 B0.25 Cl0.5 F N O Rh0.25 Te'
_chemical_formula_weight         351.94
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-19 deposited with the CCDC.    2019-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.2755(11)
_cell_length_b                   11.2755(11)
_cell_length_c                   24.219(3)
_cell_measurement_reflns_used    8643
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.126
_cell_measurement_theta_min      2.554
_cell_volume                     3079.1(6)
_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, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_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  0.0886
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28399
_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         26.446
_diffrn_reflns_theta_min         1.682
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.266
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0948 before and 0.0656 after correction. The Ratio of minimum to maximum transmission is 0.7574. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.025
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3161
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0570P)^2^+23.9166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2810
_reflns_number_total             3161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00500e1.cif
_cod_data_source_block           ph8109_0m_a
_cod_depositor_comments
'Adding full bibliography for 7049313--7049315.cif.'
_cod_original_cell_volume        3079.1(7)
_cod_original_formula_sum        'C10 H9 B0.25 Cl0.50 F N O Rh0.25 Te'
_cod_database_code               7049314
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.464
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90(6)
 0.10(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C005) \\sim Ueq, Uanis(B00H) \\sim Ueq, Uanis(C00F) \\sim Ueq,
Uanis(C007) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C007(H007), C00A(H00A), C00D(H00D), C00F(H00F), C00G(H00G)
5.b Idealised Me refined as rotating group:
 C00E(H00B,H00C,H00E)
;
_shelx_res_checksum              36759
_shelx_fab_checksum              28789
_olex2_submission_special_instructions 'No special instructions were received'