New Ni<sub>4</sub>Na<sub>2</sub>-phenylgermsesquioxane architecture: synthesis, structure and slow dynamic behaviour.
Kulakova, Alena N.; Bilyachenko, Alexey N.; Korlyukov, Alexander A.; Long, Jérôme; Levitsky, Mikhail M.; Shubina, Elena S.; Guari, Yannick; Larionova, Joulia; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6893–6897; doi:10.1039/c8dt00900g

data_7046165
_publ_section_title
;
 New Ni<sub>4</sub>Na<sub>2</sub>-phenylgermsesquioxane architecture:
 synthesis, structure and slow dynamic behaviour.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6893
_journal_page_last               6897
_journal_paper_doi               10.1039/c8dt00900g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C72 H94 Ge10 Na2 Ni4 O30, 6(C2 H6 O)'
_chemical_formula_sum            'C84 H130 Ge10 Na2 Ni4 O36'
_chemical_formula_weight         2722.60
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-04-11 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.383(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.328(3)
_cell_length_b                   22.205(4)
_cell_length_c                   16.163(3)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.28
_cell_volume                     5373.2(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            93790
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.834
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.519
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1444 before and 0.0666 after correction. The Ratio of minimum to maximum transmission is 0.4708. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       prism
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.122
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         16377
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.472
_refine_ls_R_factor_all          0.1408
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0496P)^2^+87.9075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10589
_reflns_number_total             16377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00900g2.cif
_cod_data_source_block           kl150
_cod_depositor_comments
;
         Adding full bibliography for 7046165.cif.

2024-04-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C42 H65 Ge5 Na Ni2 O18'
_cod_original_formula_weight         1361.30
_cod_original_formula_moiety         'C36 H47 Ge5 Na Ni2 O15, 3(C2 H6 O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5373.0(15)
_cod_database_code               7046165
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.498
_shelx_estimated_absorpt_t_min   0.381
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1S-H1S
 0.85 with sigma of 0.01
 O5S-C9SA = O5S-C9SB
 1.42 with sigma of 0.005
 C9SA-C10S = C9SB-C10R
 1.5 with sigma of 0.005
 O5S-C10S
 2.42 with sigma of 0.01
 O5S-C9SB = C9SB-C10R
 2.42 with sigma of 0.01
 C4SB-O2S
 2.42 with sigma of 0.01
 O2S-C4SB
 2.42 with sigma of 0.01
 O2S-C3SA = O2S-C3SB
 1.42 with sigma of 0.005
 C3SA-C4SA = C4SB-C3SB
 1.5 with sigma of 0.005
 O2S-H2SA
 0.85 with sigma of 0.01
 O2S-H2S
 0.85 with sigma of 0.01
 O5S-H5SA
 0.85 with sigma of 0.01
 O5S-H5S
 0.85 with sigma of 0.01
 C1S-H1S
 1.89033 with sigma of 0.02
 Na1-H1S
 2.757695 with sigma of 0.02
 C3SB-H2SA
 1.883938 with sigma of 0.02
 Na1-H2SA
 2.902223 with sigma of 0.02
 C3SA-H2S
 1.882971 with sigma of 0.02
 Na1-H2S
 2.758795 with sigma of 0.02
 C9SB-H5SA
 2.065622 with sigma of 0.02
 Na1-H5SA
 3.068177 with sigma of 0.02
 C9SA-H5S
 1.867325 with sigma of 0.02
 Na1-H5S
 3.010943 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C9SA) = Uiso(C9SB)
Uiso(C10R) = Uiso(C10S)
Uanis(C3SA) = Uanis(C3SB)
Uanis(C4SB) = Uanis(C4SA)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C27) = Uanis(C27A)
Uanis(C28) = Uanis(C28A)
Uanis(C29) = Uanis(C29A)
Uanis(C30) = Uanis(C30A)
Uanis(C3SB) = Uanis(C3SA)
Uanis(C4SA) = Uanis(C4SB)
4. Others
 Sof(H5SA)=Sof(C9SB)=Sof(H9SC)=Sof(H9SD)=Sof(C10R)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=1-FVAR(1)
 Sof(H5S)=Sof(C9SA)=Sof(H9SA)=Sof(H9SB)=Sof(C10S)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=FVAR(1)
 Sof(H2SA)=Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=Sof(C4SB)=Sof(H4SD)=Sof(H4SE)=
 Sof(H4SF)=1-FVAR(2)
 Sof(H2S)=Sof(C3SA)=Sof(H3SA)=Sof(H3SB)=Sof(C4SA)=Sof(H4SA)=Sof(H4SB)=
 Sof(H4SC)=FVAR(2)
 Fixed Sof: C25A(0.36807) C30A(0.36807) H30A(0.36807) C29A(0.36807)
 H29A(0.36807) C28A(0.36807) H28A(0.36807) C27A(0.36807) H27A(0.36807)
 C26A(0.36807) H26A(0.36807) C27(0.63193) H27(0.63193) C28(0.63193)
 H28(0.63193) C29(0.63193) H29(0.63193) C30(0.63193) H30(0.63193) C25(0.63193)
 C26(0.63193) H26(0.63193)
5.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C3SA(H3SA,H3SB), C3SB(H3SC,H3SD), C9SA(H9SA,H9SB), C9SB(H9SC,
 H9SD), C5S(H5SB,H5SC), C7S(H7SA,H7SB), C11S(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C30A(H30A), C29A(H29A), C28A(H28A), C27A(H27A),
 C26A(H26A), C27(H27), C28(H28), C29(H29), C30(H30), C26(H26)
5.d Fitted hexagon refined as free rotating group:
 C25A(C30A,C29A,C28A,C27A,C26A), C27(C28,C29,C30,C25,C26)
5.e Idealised Me refined as rotating group:
 C2S(H2SB,H2SC,H2SD), C4SA(H4SA,H4SB,H4SC), C4SB(H4SD,H4SE,H4SF), C10R(H10A,
 H10B,H10C), C10S(H10D,H10E,H10F), C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,H8SC),
 C12S(H12A,H12B,H12C)
5.f Idealised tetrahedral OH refined as rotating group:
 O3S(H3S), O4S(H4S), O6S(H6S)
;
_shelx_res_checksum              88424
_olex2_submission_special_instructions 'No special instructions were received'