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_7715794
_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         'C32 H14 Cu F18 N2, C H2 Cl2, C32 H12 B F24'
_chemical_formula_sum            'C65 H28 B Cl2 Cu F42 N2'
_chemical_formula_weight         1780.14
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-22 deposited with the CCDC.	2024-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                79.7320(10)
_cell_angle_beta                 73.2900(10)
_cell_angle_gamma                79.6100(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4451(4)
_cell_length_b                   14.7271(4)
_cell_length_c                   17.4381(4)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.41
_cell_volume                     3463.17(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Photon II 7 CPAD'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest Photon II 7'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_detector       'Photon II 7 CPAD'
_diffrn_radiation_monochromator  'curved 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  0.0214
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58212
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.519
_diffrn_reflns_theta_min         2.838
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'KFF MO-2KC-90'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0493 before and 0.0425 after correction.
The Ratio of minimum to maximum transmission is 0.9178.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         20956
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0631P)^2^+3.9348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18107
_reflns_number_total             20956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00822g2.cif
_cod_data_source_block           hrd132_0m_a
_cod_depositor_comments
'Adding full bibliography for 7715792--7715795.cif.'
_cod_original_cell_volume        3463.18(16)
_cod_database_code               7715794
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F41-F40 \\sim F41-F42 \\sim F40-F42
 with sigma of 0.02
 C64-F41 \\sim C64-F40 \\sim C64-F42
 with sigma of 0.01
 F41A-F40A \\sim F41A-F42A \\sim F40A-F42A
 with sigma of 0.02
 C64-F41A \\sim C64-F42A \\sim C64-F40A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F40 \\sim F41 \\sim F42 \\sim F40A \\sim F41A \\sim F42A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(F40A)=Sof(F41A)=Sof(F42A)=1-FVAR(1)
 Sof(F40)=Sof(F41)=Sof(F42)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C65(H65A,H65B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C15(H15), C17(H17), C24(H24),
 C26(H26), C34(H34), C36(H36), C38(H38), C42(H42), C44(H44), C46(H46), C50(H50),
  C52(H52), C54(H54), C58(H58), C60(H60), C62(H62)
;
_shelx_res_checksum              70888
_olex2_submission_special_instructions 'No special instructions were received'