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_7250976
_publ_section_title
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 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 Ag4 N8, 2(C H2 Cl2), 1[CH2Cl2]'
_chemical_formula_sum            'C95 H130 Ag4 Cl6 N8'
_chemical_formula_weight         2028.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 91.0530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8833(4)
_cell_length_b                   25.3326(6)
_cell_length_c                   18.9580(4)
_cell_measurement_reflns_used    9423
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      36.318
_cell_measurement_theta_min      2.518
_cell_volume                     9067.3(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            98024
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.322
_diffrn_reflns_theta_min         2.684
_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    1.078
_exptl_absorpt_correction_T_max  0.4383
_exptl_absorpt_correction_T_min  0.3912
_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    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4184
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         21859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+15.1989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17787
_reflns_number_total             21859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00912j2.cif
_cod_data_source_block           hrd286_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_database_code               7250976
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H48A(0.5) H48B(0.5) H49A(0.5) H49B(0.5)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8), C11(H11), C16(H16), C18(H18), C21(H21), C29(H29), C31(H31),
 C34(H34), C39(H39), C41(H41), C44(H44)
3.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), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B),
  C22(H22A,H22B), C23(H23A,H23B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,
 H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B),
 C40(H40A,H40B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C46(H46A,H46B),
  C48(H48A,H48B), C49(H49A,H49B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C25(H25)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 174 electrons were 
found in a volume of 1162\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
1[CH2Cl2] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29383
_shelx_fab_checksum              47845
_olex2_submission_special_instructions 'No special instructions were received'