Multinuclear copper(i) and silver(i) pyrazolates decorated with adamantyl substituents
Phan, Vo Quang Huy; Watson, Brandon T.; Noonikara-Poyil, Anurag; Duran, Katrina; Patterson, Monika R.; Dias, H. V. Rasika; CrystEngComm 27 (2025) 6987–6999; doi:10.1039/D5CE00912J

data_7250978
_publ_section_title
;
 Multinuclear copper(i) and silver(i) pyrazolates decorated with adamantyl
 substituents
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6987
_journal_page_last               6999
_journal_paper_doi               10.1039/D5CE00912J
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C92 H124 Cu4 N8, 0.6[C6H6]'
_chemical_formula_sum            'C95.6 H127.6 Cu4 N8'
_chemical_formula_weight         1643.01
_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             2025-07-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7311)
;
_audit_update_record
;
2025-07-25 deposited with the CCDC.	2025-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                73.3250(10)
_cell_angle_beta                 80.088(2)
_cell_angle_gamma                68.7620(10)
_cell_formula_units_Z            2
_cell_length_a                   15.8447(5)
_cell_length_b                   16.6587(5)
_cell_length_c                   17.2643(5)
_cell_measurement_reflns_used    9667
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.486
_cell_measurement_theta_min      2.646
_cell_volume                     4057.0(2)
_computing_cell_refinement       'SAINT V8.41 (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.41 (?, 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 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest Photon II 7'
_diffrn_measurement_method       '0.3\% \w and \f 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  0.0226
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63137
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.599
_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
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.5645
_exptl_absorpt_correction_T_min  0.5127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1746
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.093
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1183
_refine_ls_number_reflns         21760
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+4.7057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18565
_reflns_number_total             21760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00912j2.cif
_cod_data_source_block           hrd285_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7250974--7250981.cif.
;
_cod_original_formula_sum        'C95.60 H127.60 Cu4 N8'
_cod_database_code               7250978
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C38, C39, C40, C41, C42, C43, C44, C45, C46, C61, C62, C63, C64, C65, C66,
 C67, C68, C69, C74, C75, C76, C77, C78, C79, C80, C81, C82
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C1B, C1C, C1D, C1E, C1F, C1G, C1H, C1I, C1J, C1K, C1L, C1M, C1N, C1O, C1P,
 C1R, C1S, C1T, C1U, C1V, C1W, C1X, C1Y, C1Z, C2A, C2B, C2D
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
3. Uiso/Uaniso restraints and constraints
C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim
C46 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim
C68 \\sim C69 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim
C80 \\sim C81 \\sim C82: within 2A with sigma of 0.003 and sigma for terminal
atoms of 0.003 within 2A
C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G \\sim C1H \\sim C1I \\sim
C1J \\sim C1K \\sim C1L \\sim C1M \\sim C1N \\sim C1O \\sim C1P \\sim C1R \\sim
C1S \\sim C1T \\sim C1U \\sim C1V \\sim C1W \\sim C1X \\sim C1Y \\sim C1Z \\sim
C2A \\sim C2B \\sim C2D: within 2A with sigma of 0.003 and sigma for terminal
atoms of 0.003 within 2A
4. Others
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=
 Sof(H1DB)=Sof(C1E)=Sof(H1E)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(C1G)=Sof(H1G)=
 Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(C1I)=Sof(H1I)=Sof(C1J)=Sof(H1JA)=Sof(H1JB)=1-
 FVAR(1)
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=Sof(H63B)=
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66)=Sof(C67)=
 Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=Sof(H69B)=
 FVAR(1)
 Sof(C1K)=Sof(H1K)=Sof(C1L)=Sof(H1LA)=Sof(H1LB)=Sof(C1M)=Sof(H1MA)=Sof(H1MB)=
 Sof(C1N)=Sof(H1NA)=Sof(H1NB)=Sof(C1O)=Sof(H1O)=Sof(C1P)=Sof(H1PA)=Sof(H1PB)=
 Sof(C1R)=Sof(H1RA)=Sof(H1RB)=Sof(C1S)=Sof(H1S)=Sof(C1T)=Sof(H1TA)=Sof(H1TB)=1-
 FVAR(2)
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76A)=Sof(H76B)=
 Sof(C77)=Sof(H77)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=Sof(H79)=Sof(C80)=
 Sof(H80A)=Sof(H80B)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=
 FVAR(2)
 Sof(C1U)=Sof(H1U)=Sof(C1V)=Sof(H1VA)=Sof(H1VB)=Sof(C1W)=Sof(H1WA)=Sof(H1WB)=
 Sof(C1X)=Sof(H1XA)=Sof(H1XB)=Sof(C1Y)=Sof(H1Y)=Sof(C1Z)=Sof(H1ZA)=Sof(H1ZB)=
 Sof(C2A)=Sof(H2A)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C2D)=Sof(H2DA)=Sof(H2DB)=1-
 FVAR(3)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43)=Sof(C44)=
 Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8), C10(H10), C16(H16), C18(H18), C20(H20), C29(H29), C31(H31),
 C33(H33), C52(H52), C54(H54), C56(H56), C85(H85), C87(H87), C89(H89), C39(H39),
  C41(H41), C43(H43), C62(H62), C64(H64), C66(H66), C75(H75), C77(H77),
 C79(H79), C1E(H1E), C1G(H1G), C1I(H1I), C1K(H1K), C1O(H1O), C1S(H1S), C1U(H1U),
  C1Y(H1Y), C2A(H2A)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,
 H32B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C51(H51A,H51B),
 C53(H53A,H53B), C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
  C84(H84A,H84B), C86(H86A,H86B), C88(H88A,H88B), C90(H90A,H90B), C91(H91A,
 H91B), C92(H92A,H92B), C38(H38A,H38B), C40(H40A,H40B), C42(H42A,H42B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C61(H61A,H61B), C63(H63A,H63B),
  C65(H65A,H65B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C74(H74A,
 H74B), C76(H76A,H76B), C78(H78A,H78B), C80(H80A,H80B), C81(H81A,H81B),
 C82(H82A,H82B), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1F(H1FA,H1FB),
  C1H(H1HA,H1HB), C1J(H1JA,H1JB), C1L(H1LA,H1LB), C1M(H1MA,H1MB), C1N(H1NA,
 H1NB), C1P(H1PA,H1PB), C1R(H1RA,H1RB), C1T(H1TA,H1TB), C1V(H1VA,H1VB),
 C1W(H1WA,H1WB), C1X(H1XA,H1XB), C1Z(H1ZA,H1ZB), C2B(H2BA,H2BB), C2D(H2DA,H2DB)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C25(H25), C48(H48), C71(H71)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 57 electrons were 
found in a volume of 355\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
0.6[C6H6] per Asymmetric Unit 
which account for 50 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11372
_shelx_fab_checksum              81143
_olex2_submission_special_instructions 'No special instructions were received'