Synthesis and structural characterization of stable coinage metal (Cu, Ag, Au) cyclopentadienyl complexes.
Sievers, Robin; Reimann, Marc; Kub, Nico G.; Rupf, Susanne M.; Kaupp, Martin; Malischewski, Moritz; Chemical science 15 (2024) 2990–2995; doi:10.1039/d3sc06299f

data_1570785
_publ_section_title
;
 Synthesis and structural characterization of stable coinage metal (Cu,
 Ag, Au) cyclopentadienyl complexes.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              2990
_journal_page_last               2995
_journal_paper_doi               10.1039/d3sc06299f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C22 H27 Cu1 F15 P'
_chemical_formula_sum            'C22 H27 Cu F15 P'
_chemical_formula_weight         670.94
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-11-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-22 deposited with the CCDC.	2024-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2818(3)
_cell_length_b                   14.7927(5)
_cell_length_c                   19.3153(7)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    105
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.56
_cell_volume                     2638.06(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      105.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43658
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.748
_diffrn_reflns_theta_min         2.120
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0749 before and 0.0443 after correction.
The Ratio of minimum to maximum transmission is 0.8280.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.506
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         5606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1104P)^2^+4.2396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.2008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4571
_reflns_number_total             5606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06299f3.cif
_cod_data_source_block           p21_n_smr
_cod_depositor_comments
'Adding full bibliography for 1570785--1570787.cif.'
_cod_database_code               1570785
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Shared sites
{F19, F33}
{C17, C27}
{F21, F35}
{F20, F34}
{C12, C22}
{C13, C23}
{C18, C28}
{F24, F37}
{F22, F38}
{F23, F36}
{F25, F41}
{C19, C29}
{F26, F39}
{F27, F40}
{C20, C30}
{F28, F43}
{F42, F29}
{F16, F30}
{F18, F32}
{F17, F31}
{C16, C26}
{C14, C24}
{C15, C25}
{C11, C21}
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C11)
Uanis(F17) = Uanis(F4)
Uanis(F3) = Uanis(F18)
Uanis(F26) = Uanis(F12)
Uanis(F8) = Uanis(F9)
Uanis(F23) = Uanis(F22)
Uanis(C16) = Uanis(C6)
Uanis(C17) = Uanis(C7)
Uanis(C18) = Uanis(C8)
Uanis(C20) = Uanis(C10)
Uanis(C9) = Uanis(C19)
Uanis(F15) = Uanis(F42)
Uanis(Cu3) = Uanis(Cu2)
Uanis(F19) = Uanis(F33)
Uanis(F22) = Uanis(F38)
Uanis(F26) = Uanis(F39)
Uanis(C17) = Uanis(C27)
Uanis(F25) = Uanis(F41)
Uanis(F21) = Uanis(F35)
Uanis(F24) = Uanis(F37)
Uanis(F20) = Uanis(F34)
Uanis(F23) = Uanis(F36)
Uanis(C12) = Uanis(C22)
Uanis(C19) = Uanis(C29)
Uanis(C13) = Uanis(C23)
Uanis(C18) = Uanis(C28)
Uanis(C16) = Uanis(C26)
Uanis(F16) = Uanis(F30)
Uanis(F17) = Uanis(F31)
Uanis(C15) = Uanis(C25)
Uanis(F18) = Uanis(F32)
Uanis(F28) = Uanis(F43)
Uanis(F42) = Uanis(F29)
Uanis(C14) = Uanis(C24)
Uanis(F27) = Uanis(F40)
Uanis(C11) = Uanis(C21)
Uanis(C20) = Uanis(C30)
3. Others
 Fixed Sof: Cu1(0.65) F6(0.65) F8(0.65) F4(0.65) F7(0.65) F13(0.65) F12(0.65)
 F9(0.65) F11(0.65) F3(0.65) F1(0.65) F14(0.65) F10(0.65) F5(0.65) F2(0.65)
 C3(0.65) C2(0.65) C1(0.65) C5(0.65) C7(0.65) C10(0.65) C4(0.65) C8(0.65)
 C9(0.65) C6(0.65) Cu2(0.175) F25(0.175) F20(0.175) F26(0.175) F27(0.175)
 F16(0.175) F23(0.175) F24(0.175) F28(0.175) F22(0.175) F21(0.175) F18(0.175)
 F17(0.175) F19(0.175) F42(0.175) C19(0.175) C16(0.175) C11(0.175) C12(0.175)
 C15(0.175) C14(0.175) C20(0.175) C13(0.175) C17(0.175) C18(0.175) Cu3(0.175)
 F41(0.175) F34(0.175) F39(0.175) F30(0.175) F36(0.175) F37(0.175) F43(0.175)
 F38(0.175) F35(0.175) F32(0.175) F31(0.175) F33(0.175) F29(0.175) C29(0.175)
 C26(0.175) C21(0.175) C22(0.175) F40(0.175) C25(0.175) C24(0.175) C30(0.175)
 C23(0.175) C27(0.175) C28(0.175)
4.a Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C35(H35A,
 H35B,H35C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              42504
_olex2_submission_special_instructions 'No special instructions were received'