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_7049313
_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         'C108 H150 N6 O6 Te6, 4(C7 H8)'
_chemical_formula_sum            'C136 H182 N6 O6 Te6'
_chemical_formula_weight         2762.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-26 deposited with the CCDC.    2019-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.272(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.067(2)
_cell_length_b                   20.129(2)
_cell_length_c                   16.9559(18)
_cell_measurement_reflns_used    9415
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.504
_cell_measurement_theta_min      2.291
_cell_volume                     6480.1(12)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            190828
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_min         1.966
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0500 before and 0.0439 after correction. The Ratio of minimum to maximum transmission is 0.9341. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         13244
_refine_ls_number_restraints     654
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+17.0378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11027
_reflns_number_total             13244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00500e1.cif
_cod_data_source_block           acmacrocycle_a
_cod_depositor_comments
'Adding full bibliography for 7049313--7049315.cif.'
_cod_original_cell_volume        6480.2(12)
_cod_database_code               7049313
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.897
_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. 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
3. Others
 Fixed Sof: C0AA(0.5) H0AB(0.5) H0AC(0.5) H0AD(0.5) C1AA(0.5) H1AB(0.5)
 H1AC(0.5) H1AD(0.5) C2AA(0.5) H2AB(0.5) H2AC(0.5) H2AD(0.5) C8A(0.5) H8AA(0.5)
 H8AB(0.5) H8AC(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) C5A(0.5) H5AA(0.5)
 H5AB(0.5) H5AC(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00G(H00G), C2(H2), C00I(H00I), C6(H6), C00S(H00S), C00U(H00U),
 C00V(H00V), C00W(H00W), C00X(H00X), C10(H10), C01B(H01J), C01N(H4AA),
 C01P(H6AA), C01R(H9AA), C01S(H0BA), C01U(H2BA), C01V(H3BA), C01W(H4BA),
 C01Y(H5BA), C01Z(H1BA), C020(H020)
4.b Idealised Me refined as rotating group:
 C00J(H00A,H00B,H00D), C011(H01A,H01B,H01C), C016(H01D,H01E,H01F), C4(H4A,H4B,
 H4C), C018(H01G,H01H,H01I), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C01D(H01K,
 H01L,H01M), C01E(H01N,H01O,H01P), C01F(H01Q,H01R,H01S), C01G(H01T,H01U,H01V),
 C01H(H01W,H01X,H01Y), C01I(H01Z,H,HA), C01K(H01,HB,HC), C01L(H0AA,HD,HE),
 C01M(H1AA,HF,HG), C01Q(H2AA,HH,HI), C01T(H3AA,HJ,HK), C021(H02D,H02E,H02F),
 C022(H02A,H02B,H02C), C0AA(H0AB,H0AC,H0AD), C1AA(H1AB,H1AC,H1AD), C2AA(H2AB,
 H2AC,H2AD), C8A(H8AA,H8AB,H8AC), C7A(H7AA,H7AB,H7AC), C5A(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              10451
_olex2_submission_special_instructions 'No special instructions were received'