Detailed structural and spectroscopic elucidation of ferrocenium coupled N-heterocyclic carbene gold(I) complexes.
Reinhard, Garrett L.; Jayaraman, Selvakumar; Prybil, Joshua W.; Arambula, Jonathan F.; Arumugam, Kuppuswamy; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1533–1541; doi:10.1039/d1dt03174k

data_7709255
_publ_section_title
;
 Detailed structural and spectroscopic elucidation of ferrocenium coupled
 N-heterocyclic carbene gold(I) complexes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1533
_journal_page_last               1541
_journal_paper_doi               10.1039/d1dt03174k
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C46 H48 Au Fe2 N4, B F4'
_chemical_formula_sum            'C46 H48 Au B F4 Fe2 N4'
_chemical_formula_weight         1052.40
_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_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-13 deposited with the CCDC.	2021-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.344(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.798(2)
_cell_length_b                   23.649(4)
_cell_length_c                   15.577(3)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.90
_cell_volume                     4333.7(13)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Apex3 v2017.3-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.9949
_diffrn_measured_fraction_theta_max 0.9949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54241
_diffrn_reflns_theta_full        28.2939
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.71
_diffrn_source                   'sealed tube X-ray source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.092
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1359 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.6959.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.6129
_exptl_crystal_description       needle
_exptl_crystal_F_000             2092.4507
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.7740
_refine_diff_density_min         -1.3783
_refine_diff_density_rms         0.1529
_refine_ls_d_res_high            0.7497
_refine_ls_d_res_low             7.5178
_refine_ls_goodness_of_fit_ref   1.0561
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    82
_refine_ls_number_parameters     529
_refine_ls_number_reflns         10721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0561
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+6.3633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8333
_reflns_number_total             10721
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03174k2.cif
_cod_data_source_block           19SW013LT_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7709255--7709257.cif.
;
_cod_original_cell_volume        4333.7(14)
_cod_database_code               7709255
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C36(H36a,H36b)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C2(H2), C3(H3), C31(H31), C26(H26), C25(H25), C6(H6), C17(H17),
 C8(H8), C21(H21), C29(H29), C38(H38), C41(H41), C39(H39), C15(H15), C40(H40),
 C16(H16), C22(H22), C44(H44), C43(H43), C20(H20), C45(H45), C42(H42), C46(H46)
2.d Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C35(H35a,H35b,H35c), C10(H10a,H10b,H10c), C34(H34a,H34b,
 H34c), C12(H12a,H12b,H12c), C11(H11a,H11b,H11c)
;
_olex2_submission_special_instructions 'No special instructions were received'