Synthons for carbide complex chemistry.
Reinholdt, Anders; Hill, Anthony F.; Bendix, Jesper; Chemical communications (Cambridge, England) 54 (2018) 5708–5711; doi:10.1039/c8cc03596b

data_7121653
_publ_section_title
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 Synthons for carbide complex chemistry.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5708
_journal_page_last               5711
_journal_paper_doi               10.1039/c8cc03596b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C25 H43 Cl4 N4 O P Pt Ru, 3(C H Cl3)'
_chemical_formula_sum            'C28 H46 Cl13 N4 O P Pt Ru'
_chemical_formula_weight         1242.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-02-15 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6569(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4348(7)
_cell_length_b                   11.4929(6)
_cell_length_c                   27.5886(14)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.319
_cell_measurement_theta_min      2.295
_cell_volume                     4427.9(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            85935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.295
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.347
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1404 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.6484.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          1.125
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.983
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10147
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0254P)^2^+13.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9061
_reflns_number_total             10147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03596b2.cif
_cod_data_source_block           mo_d8v3059_0m-1
_cod_depositor_comments
'Adding full bibliography for 7121645--7121655.cif.'
_cod_database_code               7121653
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.084
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All Cl(H,H) groups
2. Restrained distances
 O1-H1a = O1-H1b
 0.88 with sigma of 0.01
 Cl7A-C41A \\sim Cl5A-C41A \\sim Cl6A-C41A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(Cl7A) = Uiso(C41A) = Uiso(Cl6A) = Uiso(Cl5A)
4. Others
 Sof(C28A)=Sof(Hw)=Sof(Cl14)=Sof(Cl15)=Sof(Cl16)=1-FVAR(1)
 Sof(Cl12)=Sof(Cl11)=Sof(Cl13)=Sof(C28)=Sof(H28)=FVAR(1)
 Sof(Pt1A)=Sof(Cl4A)=Sof(N3A)=Sof(N2A)=Sof(H2Aa)=Sof(C20A)=Sof(Hx)=Sof(C21A)=
 Sof(Hy)=Sof(C22A)=Sof(Hz)=Sof(N1A)=Sof(C25A)=Sof(H25A)=Sof(C24A)=Sof(H24A)=
 Sof(C23A)=Sof(H23A)=Sof(N4A)=Sof(H4Aa)=1-FVAR(2)
 Sof(Pt1)=Sof(Cl4)=Sof(N3)=Sof(N4)=Sof(H4)=Sof(N1)=Sof(C21)=Sof(Hb)=Sof(N2)=
 Sof(H2a)=Sof(C24)=Sof(H24)=Sof(C20)=Sof(Hh)=Sof(C23)=Sof(H23)=Sof(C25)=
 Sof(H25)=Sof(C22)=Sof(Hv)=FVAR(2)
 Sof(H14a)=Sof(Hk)=Sof(Hl)=Sof(H18a)=Sof(Hp)=Sof(C19A)=Sof(H19c)=Sof(H19d)=
 Sof(C17A)=Sof(H0aa)=Sof(H1aa)=Sof(C16A)=Sof(H3aa)=Sof(H5aa)=1-FVAR(3)
 Sof(H14)=Sof(C19)=Sof(H19b)=Sof(H19a)=Sof(C17)=Sof(He)=Sof(Hf)=Sof(Hi)=
 Sof(Hj)=Sof(C16)=Sof(Hm)=Sof(Hn)=Sof(Ho)=Sof(H18)=FVAR(3)
 Sof(H27a)=Sof(Cl17)=1-FVAR(4)
 Sof(Cl10)=Sof(H27)=FVAR(4)
 Fixed Sof: Cl6(0.8) Cl7(0.8) Cl5(0.8) C41(0.8) Hg(0.8) C41A(0.2) H41A(0.2)
 Cl7A(0.2) Cl6A(0.2) Cl5A(0.2)
5.a Ternary CH refined with riding coordinates:
 C14(H14a), C14(H14), C2(H2), C27(H27a), C27(H27), C28(H28), C41(Hg), C8(Hu),
 C28A(Hw), C41A(H41A)
5.b Secondary CH2 refined with riding coordinates:
 C13(H,Ha), C9(H9a,H9b), C19(H19b,H19a), C3(H3a,H3b), C4(H4a,H4b), C6(H6a,H6b),
  C12(Hc,Hd), C17(He,Hf), C5(H5a,H5b), C15(Hi,Hj), C15(Hk,Hl), C16(Hm,Hn),
 C7(H7a,H7b), C18(Ho,H18), C18(H18a,Hp), C11(Hq,Hr), C10(Hs,Ht), C19A(H19c,
 H19d), C17A(H0aa,H1aa), C16A(H3aa,H5aa)
5.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C21(Hb), N2(H2a), C24(H24), C20(Hh), C23(H23), C25(H25), C22(Hv),
 N2A(H2Aa), C20A(Hx), C21A(Hy), C22A(Hz), C25A(H25A), C24A(H24A), C23A(H23A),
 N4A(H4Aa)
;
_shelx_res_checksum              39206
_olex2_submission_special_instructions 'No special instructions were received'