Synthesis and characterization of heterometallic complexes involving coinage metals and isoelectronic Fe(CO)<sub>5</sub>, [Mn(CO)<sub>5</sub>]<sup>-</sup> and [Fe(CO)<sub>4</sub>CN]<sup>-</sup> ligands.
Ponduru, Tharun Teja; Wang, Guocang; Manoj, Sai; Pan, Sudip; Zhao, Lili; Frenking, Gernot; Dias, H. V. Rasika; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8566–8581; doi:10.1039/d0dt01590c

data_1558140
_publ_section_title
;
 Synthesis and characterization of heterometallic complexes involving
 coinage metals and isoelectronic Fe(CO)<sub>5</sub>,
 [Mn(CO)<sub>5</sub>]<sup>-</sup> and [Fe(CO)<sub>4</sub>CN]<sup>-</sup>
 ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8566
_journal_page_last               8581
_journal_paper_doi               10.1039/d0dt01590c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C32 H38 Ag Mn N2 O5, C4 H8 O'
_chemical_formula_sum            'C36 H46 Ag Mn N2 O6'
_chemical_formula_weight         765.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-04-27 deposited with the CCDC.	2020-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6971(6)
_cell_length_b                   19.4845(13)
_cell_length_c                   21.3902(14)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.19
_cell_measurement_theta_min      3.14
_cell_volume                     3624.8(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker D8 Quest with a Photon 100 CMOS detector'
_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  0.0296
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51706
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.505
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.4353
_exptl_absorpt_correction_T_min  0.3921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0584 before and 0.0526 after correction. The Ratio of minimum to maximum transmission is 0.9008. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6180
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0297P)^2^+1.8026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5570
_reflns_number_total             6180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01590c2.cif
_cod_data_source_block           rad569_0m_a
_cod_depositor_comments
'Adding full bibliography for 1558136--1558141.cif.'
_cod_database_code               1558140
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.850
_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. Restrained distances
 C22-C21 \\sim C21-C20 \\sim C20-C19
 with sigma of 0.02
 O5-C22 \\sim O5-C19
 with sigma of 0.02
 O5-C21 \\sim O5-C20
 with sigma of 0.04
 C21-C19 \\sim C22-C20
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O5 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O5, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O5(0.5) C19(0.5) H19A(0.5) H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 C21(0.5) H21A(0.5) H21B(0.5) C22(0.5) H22A(0.5) H22B(0.5)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              22221
_olex2_submission_special_instructions 'No special instructions were received'