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_7049315
_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         'C72 H100 N4 O4 Pt Te4, 2(B F4)'
_chemical_formula_sum            'C72 H100 B2 F8 N4 O4 Pt Te4'
_chemical_formula_weight         1964.66
_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     dual
_audit_creation_date             2019-01-30
_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.    2019-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.411(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8287(7)
_cell_length_b                   31.4108(17)
_cell_length_c                   20.5844(11)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.269
_cell_measurement_theta_min      2.192
_cell_volume                     8941.0(8)
_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      100.15
_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  0.1279
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            223351
_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         27.022
_diffrn_reflns_theta_min         1.183
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0631 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.9132. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.373
_refine_diff_density_min         -2.149
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         19494
_refine_ls_number_restraints     919
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0268P)^2^+61.4496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12960
_reflns_number_total             19494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00500e1.cif
_cod_data_source_block           0m_a
_cod_depositor_comments
'Adding full bibliography for 7049313--7049315.cif.'
_cod_database_code               7049315
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.623
_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. Restrained distances
 C51-C54 \\sim C51-C1A
 with sigma of 0.02
 C3AA-C52 \\sim C2A-C53
 with sigma of 0.02
 C51-C3AA \\sim C51-C2A
 with sigma of 0.04
 C51-C52 \\sim C51-C53
 with sigma of 0.04
 C02B-C69 \\sim C70-C69
 with sigma of 0.02
 C69-C02M \\sim C69-C71
 with sigma of 0.02
 C69-C02P \\sim C69-C72
 with sigma of 0.02
3. 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
4. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=1-FVAR(1)
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=
 Sof(H3AC)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(1)
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=1-FVAR(2)
 Sof(C02B)=Sof(H02A)=Sof(H02B)=Sof(H02C)=Sof(C02M)=Sof(H02D)=Sof(H02E)=
 Sof(H02F)=Sof(C02P)=Sof(H02G)=Sof(H02H)=Sof(H02I)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C2(H2), C28(H28), C24(H24), C6(H6), C38(H38), C10(H10), C60(H60),
 C26(H26), C46(H46), C64(H64), C8(H8), C56(H56), C42(H42), C62(H62), C44(H44)
5.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C58(H58A,H58B,H58C), C4(H4A,H4B,H4C), C40(H40A,H40B,
 H40C), C13(H13A,H13B,H13C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C32(H32A,
 H32B,H32C), C14(H14A,H14B,H14C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C),
 C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C02B(H02A,H02B,H02C), C36(H36A,H36B,
 H36C), C67(H67A,H67B,H67C), C17(H17A,H17B,H17C), C66(H66A,H66B,H66C), C68(H68A,
 H68B,H68C), C16(H16A,H16B,H16C), C02M(H02D,H02E,H02F), C50(H50A,H50B,H50C),
 C48(H48A,H48B,H48C), C02P(H02G,H02H,H02I), C49(H49A,H49B,H49C), C54(H54A,H54B,
 H54C), C3AA(H3AA,H3AB,H3AC), C52(H52A,H52B,H52C), C1A(H1AA,H1AB,H1AC),
 C2A(H2AA,H2AB,H2AC), C53(H53A,H53B,H53C), C72(H72A,H72B,H72C), C71(H71A,H71B,
 H71C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              14989
_shelx_fab_checksum              30108
_olex2_submission_special_instructions 'No special instructions were received'