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_7250977
_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         'C48 H69 Ag3 N6'
_chemical_formula_sum            'C48 H69 Ag3 N6'
_chemical_formula_weight         1053.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-25 deposited with the CCDC.	2025-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.890(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9738(17)
_cell_length_b                   12.7162(15)
_cell_length_c                   23.893(3)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      30.25
_cell_measurement_theta_min      2.30
_cell_volume                     4525.4(9)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.98
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector       'PHOTON II 7 CPAD'
_diffrn_radiation_monochromator  'mirror optics'
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51816
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.525
_diffrn_reflns_theta_min         1.367
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1005 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.8768.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.927
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.100
_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     550
_refine_ls_number_reflns         13405
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0352P)^2^+3.7458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11244
_reflns_number_total             13405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00912j2.cif
_cod_data_source_block           dia14_0m_a
_cod_depositor_comments
'Adding full bibliography for 7250974--7250981.cif.'
_cod_database_code               7250977
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.700
_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
 C30-C19 \\sim C30A-C19
 with sigma of 0.005
 C31-C30 \\sim C32-C30 \\sim C32A-C30A \\sim C30A-C31A
 with sigma of 0.005
3. Rigid bond restraints
 C30, C30A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C30 \\sim C30A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.005 within 1.7A
5. Others
 Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=1-FVAR(1)
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32A)=
 Sof(H32D)=Sof(H32E)=Sof(H32F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8), C11(H11), C14(H14), C22(H22), C24(H24), C27(H27), C38(H38),
 C40(H40), C43(H43), C46(H46), C30(H30), C30A(H30A)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C13(H13A,H13B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B),
  C28(H28A,H28B), C29(H29A,H29B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,
 H41B), C42(H42A,H42B), C44(H44A,H44B), C45(H45A,H45B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C18(H18), C34(H34)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C31A(H31D,H31E,H31F),
 C32A(H32D,H32E,H32F)
;
_shelx_res_checksum              40539
_olex2_submission_special_instructions 'No special instructions were received'