Coinage metal-ethylene complexes of sterically demanding 1,10-phenanthroline ligands.
Karade, Deepika V.; Phan, Vo Quang Huy; Dias, H. V. Rasika; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10426–10433; doi:10.1039/d4dt00822g

data_7715792
_publ_section_title
;
 Coinage metal-ethylene complexes of sterically demanding
 1,10-phenanthroline ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10426
_journal_page_last               10433
_journal_paper_doi               10.1039/d4dt00822g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C44 H56 Cu N2, C H2 Cl2, F6 Sb'
_chemical_formula_sum            'C45 H58 Cl2 Cu F6 N2 Sb'
_chemical_formula_weight         997.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-22 deposited with the CCDC.	2024-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                88.4970(10)
_cell_angle_beta                 87.2490(10)
_cell_angle_gamma                78.8350(10)
_cell_formula_units_Z            2
_cell_length_a                   9.1342(9)
_cell_length_b                   12.9011(12)
_cell_length_c                   19.4966(19)
_cell_measurement_reflns_used    9445
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      30.40
_cell_measurement_theta_min      2.27
_cell_volume                     2251.1(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.98
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'Bruker ApexII'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart ApexII'
_diffrn_measurement_method       '0.3\ \w and 0.3\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker ApexII'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.539
_diffrn_reflns_theta_min         1.609
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0636 before and 0.0336 after correction.
The Ratio of minimum to maximum transmission is 0.9055.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.634
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         12957
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0926P)^2^+2.5862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10102
_reflns_number_total             12957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00822g2.cif
_cod_data_source_block           dia94_0m_a
_cod_depositor_comments
'Adding full bibliography for 7715792--7715795.cif.'
_cod_database_code               7715792
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.665
_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
 Sb2-F7 = Sb2-F8 = Sb2-F10 = Sb2-F12
 1.88 with sigma of 0.02
 Sb2-F9 = Sb2-F11
 1.87 with sigma of 0.02
 C37-C31 \\sim C37A-C31
 with sigma of 0.02
 C45-C37 \\sim C45A-C37A \\sim C38-C37 \\sim C38A-C37A
 with sigma of 0.02
 F7-F8 \\sim F7-F9 \\sim F7-F10 \\sim F7-F11 \\sim F8-F9 \\sim F8-F11 \\sim
F8-F12 \\sim F9-F10 \\sim F9-F12 ~
 F10-F11 \\sim F10-F12 \\sim F11-F12
 with sigma of 0.04
 Sb2-F7 \\sim Sb2-F8 \\sim Sb2-F9 \\sim Sb2-F10 \\sim Sb2-F11 \\sim Sb2-F12
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Sb2 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C38 \\sim C37 \\sim C45 \\sim C37A \\sim C38A \\sim C45A: within 2A with sigma
of 0.008 and sigma for terminal atoms of 0.008 within 2A
4. Rigid body (RIGU) restrains
 Sb2, F7, F8, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(H45C)=1-FVAR(1)
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C45A)=
 Sof(H45D)=Sof(H45E)=Sof(H45F)=FVAR(1)
 Sof(Sb2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(2)
 Sof(Sb)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C25(H25), C34(H34), C39(H39), C37(H37), C37A(H37A)
6.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C15(H15), C17(H17), C30(H30),
 C32(H32)
6.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C38(H38A,H38B,H38C),
 C45(H45A,H45B,H45C), C38A(H38D,H38E,H38F), C45A(H45D,H45E,H45F)
;
_shelx_res_checksum              82048
_olex2_submission_special_instructions 'No special instructions were received'