Octahedral molybdenum iodide clusters with pyrazole or pyrazolate ligands.
Kozlova, Ksenia S.; Berezin, Alexey S.; Kuratieva, Natalia V.; Shestopalov, Michael A.; Ivanov, Anton A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15959–15967; doi:10.1039/d4dt01831a

data_7716991
_publ_section_title
;
 Octahedral molybdenum iodide clusters with pyrazole or pyrazolate
 ligands.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15959
_journal_page_last               15967
_journal_paper_doi               10.1039/d4dt01831a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H24 I8 Mo6 N12, 4(N O3), 4(C3 H4 N2)'
_chemical_formula_sum            'C30 H40 I8 Mo6 N24 O12'
_chemical_formula_weight         2519.70
_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     direct
_audit_creation_date             2023-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-06-19 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0559(3)
_cell_length_b                   11.5527(3)
_cell_length_c                   24.1189(6)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.26
_cell_measurement_theta_min      2.46
_cell_volume                     3020.46(14)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            69472
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         34.355
_diffrn_reflns_theta_min         2.215
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.368
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.5734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0766 before and 0.0540 after correction.
The Ratio of minimum to maximum transmission is 0.7678.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.770
_exptl_crystal_description       plate
_exptl_crystal_F_000             2320
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.377
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.00042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         12673
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+2.1499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9790
_reflns_number_total             12673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01831a2.cif
_cod_data_source_block           juc1407a
_cod_depositor_comments
'Adding full bibliography for 7716988--7716991.cif.'
_cod_database_code               7716991
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.413
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O3A) \\sim Ueq: with sigma of
0.0012 and sigma for terminal atoms of 0.0012
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
Uanis(O3A) = Uanis(O3B)
Uanis(N1A) = Uanis(N1B)
3. Others
 Sof(O1B)=Sof(N1B)=Sof(O3B)=Sof(O2B)=1-FVAR(1)
 Sof(O2A)=Sof(O3A)=Sof(O1A)=Sof(N1A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 N11S(H11S), N12(H12), N21S(H21S), C21S(H21A), N22(H22), N32(H32), C11S(H11A),
 C11(H11), C12(H12A), C12S(H12S), C13(H13), C13S(H13S), C21(H21), C22S(H22S),
 C22(H22A), C23S(H23S), C23(H23), C31(H31), C32(H32A), C33(H33)
;
_shelx_res_checksum              23720
_shelx_hkl_checksum              10608
_olex2_submission_special_instructions 'No special instructions were received'