Chemoselective synthesis of heterobimetallic bis-NHC complexes.
Dutschke, Patrick D.; Bente, Stefanie; Daniliuc, Constantin G.; Kinas, Jenny; Hepp, Alexander; Hahn, F. Ekkehardt; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14388–14392; doi:10.1039/d0dt03369c

data_7705648
_publ_section_title
;
 Chemoselective synthesis of heterobimetallic bis-NHC complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14388
_journal_page_last               14392
_journal_paper_doi               10.1039/d0dt03369c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C45 H41 Cl N4 P Pt, C Cl2, F6 P'
_chemical_formula_sum            'C46 H41 Cl3 F6 N4 P2 Pt'
_chemical_formula_weight         1127.21
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-05 deposited with the CCDC.	2020-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.1760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3321(3)
_cell_length_b                   25.8698(6)
_cell_length_c                   16.9685(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    99.91
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.34
_cell_volume                     4910.8(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.91
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74126
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.048
_diffrn_reflns_theta_min         1.983
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.144
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1546 before and 0.0698 after correction.
The Ratio of minimum to maximum transmission is 0.8173.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       needle
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.826
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         11862
_refine_ls_number_restraints     579
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0231P)^2^+17.6127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9873
_reflns_number_total             11862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03369c2.cif
_cod_data_source_block           structure
_cod_depositor_comments
'Adding full bibliography for 7705647--7705651.cif.'
_cod_database_code               7705648
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.287
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C100-Cl50 \\sim C100-Cl5A \\sim C100-Cl5B
 with sigma of 0.01
3. Rigid bond restraints
 C1, C3, C23, C24, C24', C25, C25', C26, C28'
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C1 \\sim C3 \\sim C23 \\sim C24 \\sim C24' \\sim C25 \\sim C25' \\sim C26 \\sim
C28': within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(Cl5B)=1-FVAR(1)
 Sof(Cl5A)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C17(H17A,H17B)
7.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C21(H21), C22(H22), C25(H25), C25'(H25'), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C28'(H28A,H28B,H28C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97401
_shelx_fab_checksum              26095
_olex2_submission_special_instructions 'No special instructions were received'