Quadruple bridged-carbonate supported dodecanuclear [Ni8Ca4] coordination cluster
Kajal,; Vinayak, Richa; Gómez-García, Carlos J.; Benmansour, Samia; Nayek, Hari Pada; New Journal of Chemistry 48 (2024) 3239–3246; doi:10.1039/D3NJ05217F

data_7062973
_publ_section_title
;
 Quadruple bridged-carbonate supported dodecanuclear [Ni8Ca4] coordination
 cluster
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3239
_journal_page_last               3246
_journal_paper_doi               10.1039/D3NJ05217F
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety
'C129.326 H113 Ca4 N20.442 Ni8 O63, 4.1(H2 O), C3 H7 N O, 16[H2O]'
_chemical_formula_sum            'C132.326 H160.2 Ca4 N21.442 Ni8 O84.1'
_chemical_formula_weight         4026.600
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_symmetry_Int_Tables_number      86
_audit_creation_date             2024-01-03
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.12.20 svn.rf89b8cd1 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-01-11 deposited with the CCDC.	2024-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.8062(4)
_cell_length_b                   17.8062(4)
_cell_length_c                   27.5424(8)
_cell_measurement_reflns_used    5208
_cell_measurement_temperature    373.00(10)
_cell_measurement_theta_max      27.3060
_cell_measurement_theta_min      2.4840
_cell_volume                     8732.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      373.15
_diffrn_detector_area_resol_mean 16.0606
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9907
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -82.00   0.00   1.00   52.38    --  -16.80 -38.00 -60.00   82
  2  \w    -42.00  -9.00   1.00   52.38    --  -16.80  77.00 -60.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9907
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            23307
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9907
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       prism
_exptl_crystal_F_000             4173.186
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.8120
_refine_diff_density_min         -0.6780
_refine_diff_density_rms         0.1286
_refine_ls_d_res_high            0.7829
_refine_ls_d_res_low             9.2924
_refine_ls_goodness_of_fit_ref   1.0586
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    82
_refine_ls_number_parameters     720
_refine_ls_number_reflns         9448
_refine_ls_number_restraints     638
_refine_ls_restrained_S_all      1.0216
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+9.1499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                6273
_reflns_number_total             9448
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj05217f2.cif
_cod_data_source_block           rv_1061
_cod_depositor_comments          'Adding full bibliography for 7062973.cif.'
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7062973
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O16-C30
 1.32 with sigma of 0.01
 Ni1-O16
 2 with sigma of 0.01
 C1a-O17
 1.22 with sigma of 0.02
 C1a-N6
 1.36 with sigma of 0.02
 N6-C1b
 1.45 with sigma of 0.02
 N6-C1c
 1.46 with sigma of 0.02
 C1a-C1b
 2.46 with sigma of 0.04
 C1a-C1c
 2.45 with sigma of 0.04
 C30-N5 \\sim C30a-N5a
 with sigma of 0.02
 C30-O16 \\sim C30a-O16a
 with sigma of 0.02
 C31-N5 \\sim C31a-N5a
 with sigma of 0.02
 C32-N5 \\sim C32a-N5a
 with sigma of 0.02
 Ni1-O16 \\sim Ni1-O16a
 with sigma of 0.02
 C30-C31 \\sim C30a-C31a
 with sigma of 0.04
 C30-C32 \\sim C30a-C32a
 with sigma of 0.04
 C30-Ni1 \\sim C30a-Ni1
 with sigma of 0.04
 C31-C32 \\sim C31a-C32a
 with sigma of 0.04
 N5-O16 \\sim N5a-O16a
 with sigma of 0.04
 N6-C1b \\sim N6-C1c
 with sigma of 0.02
 C15-C16 \\sim C15a-C16a
 with sigma of 0.02
 C15-C20 \\sim C15a-C20a
 with sigma of 0.02
 C15-O6 \\sim C15a-O6a
 with sigma of 0.02
 C16-H16 \\sim C16a-H16a
 with sigma of 0.02
 C16-C17 \\sim C16a-C17a
 with sigma of 0.02
 C17-H17 \\sim C17a-H17a
 with sigma of 0.02
 C17-C18 \\sim C17a-C18a
 with sigma of 0.02
 C18-C19 \\sim C18a-C19a
 with sigma of 0.02
 C18-N4 \\sim C18a-N4a
 with sigma of 0.02
 C19-H19 \\sim C19a-H19a
 with sigma of 0.02
 C19-C20 \\sim C19a-C20a
 with sigma of 0.02
 C20-N3 \\sim C20a-N3a
 with sigma of 0.02
 C21-C22
 with sigma of 0.02
 C21-N3
 with sigma of 0.02
 N3-Ni2 \\sim N3a-Ni2
 with sigma of 0.02
 Ni1-O6 \\sim Ni1-O6a
 with sigma of 0.02
 Ni2-O6 \\sim Ni2-O6a
 with sigma of 0.02
 N4-O9 \\sim N4a-O9a
 with sigma of 0.02
 N4-O10 \\sim N4a-O10a
 with sigma of 0.02
 C15-H16 \\sim C15a-H16a
 with sigma of 0.04
 C15-C17 \\sim C15a-C17a
 with sigma of 0.04
 C15-C19 \\sim C15a-C19a
 with sigma of 0.04
 C15-N3 \\sim C15a-N3a
 with sigma of 0.04
 C15-Ni1 \\sim C15a-Ni1
 with sigma of 0.04
 C15-Ni2 \\sim C15a-Ni2
 with sigma of 0.04
 C16-H17 \\sim C16a-H17a
 with sigma of 0.04
 C16-C18 \\sim C16a-C18a
 with sigma of 0.04
 C16-C20 \\sim C16a-C20a
 with sigma of 0.04
 C16-O6 \\sim C16a-O6a
 with sigma of 0.04
 H16-C17 \\sim H16a-C17a
 with sigma of 0.04
 C17-C19 \\sim C17a-C19a
 with sigma of 0.04
 C17-N4 \\sim C17a-N4a
 with sigma of 0.04
 H17-C18 \\sim H17a-C18a
 with sigma of 0.04
 C18-H19 \\sim C18a-H19a
 with sigma of 0.04
 C18-C20 \\sim C18a-C20a
 with sigma of 0.04
 C18-O9 \\sim C18a-O9a
 with sigma of 0.04
 C18-O10 \\sim C18a-O10a
 with sigma of 0.04
 C19-N3 \\sim C19a-N3a
 with sigma of 0.04
 C19-N4 \\sim C19a-N4a
 with sigma of 0.04
 H19-C20 \\sim H19a-C20a
 with sigma of 0.04
 C20-C21
 with sigma of 0.04
 C20-Ni2 \\sim C20a-Ni2
 with sigma of 0.04
 C20-O6 \\sim C20a-O6a
 with sigma of 0.04
 C21-Ni2
 with sigma of 0.04
 C22-N3 \\sim C22-N3a
 with sigma of 0.04
 O9-O10 \\sim O9a-O10a
 with sigma of 0.04
 C33-C2a
 with sigma of 0.02
 C33-C6a
 with sigma of 0.02
 C33-O1a
 with sigma of 0.02
 C2a-C3a
 with sigma of 0.02
 C3a-C4a
 with sigma of 0.02
 C4a-C5a
 with sigma of 0.02
 C4a-N2a
 with sigma of 0.02
 C5a-C6a
 with sigma of 0.02
 C6a-N1a
 with sigma of 0.02
 C7a-C8a
 with sigma of 0.02
 C7a-N1a
 with sigma of 0.02
 C8a-C9a
 with sigma of 0.02
 C8a-C13a
 with sigma of 0.02
 C9a-C10a
 with sigma of 0.02
 C10a-C11a
 with sigma of 0.02
 C11a-C12a
 with sigma of 0.02
 C12a-C13a
 with sigma of 0.02
 C12a-O3a
 with sigma of 0.02
 C13a-O2a
 with sigma of 0.02
 C14a-O3a
 with sigma of 0.02
 N2a-O4a
 with sigma of 0.02
 N2a-O5a
 with sigma of 0.02
 C33-C3a
 with sigma of 0.04
 C33-C5a
 with sigma of 0.04
 C33-N1a
 with sigma of 0.04
 C2a-C4a
 with sigma of 0.04
 C2a-C6a
 with sigma of 0.04
 C2a-O1a
 with sigma of 0.04
 C3a-C5a
 with sigma of 0.04
 C3a-N2a
 with sigma of 0.04
 C4a-C6a
 with sigma of 0.04
 C4a-O4a
 with sigma of 0.04
 C4a-O5a
 with sigma of 0.04
 C5a-N1a
 with sigma of 0.04
 C5a-N2a
 with sigma of 0.04
 C6a-C7a
 with sigma of 0.04
 C6a-O1a
 with sigma of 0.04
 C7a-C9a
 with sigma of 0.04
 C7a-C13a
 with sigma of 0.04
 C8a-C10a
 with sigma of 0.04
 C8a-C12a
 with sigma of 0.04
 C8a-N1a
 with sigma of 0.04
 C8a-O2a
 with sigma of 0.04
 C9a-C11a
 with sigma of 0.04
 C9a-C13a
 with sigma of 0.04
 C10a-C12a
 with sigma of 0.04
 C11a-C13a
 with sigma of 0.04
 C11a-O3a
 with sigma of 0.04
 C12a-C14a
 with sigma of 0.04
 C12a-O2a
 with sigma of 0.04
 C13a-O3a
 with sigma of 0.04
 O4a-O5a
 with sigma of 0.04
3. Restrained planarity
 C1a, O17, N6, C1b, C1c
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1a \\sim O17 \\sim N6 \\sim C1b \\sim C1c: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O20 \\sim O19 \\sim O18: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(O16) = Uanis(O16a)
5. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C16, C15, C20, C19, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, Ca1, O15, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Ca1, O15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Ca1, O8, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O16, C30, N5, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5a, C30a, O16a, C31a, C32a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1a, O17, N6, C1b, C1c
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, C15, C16, C17, C18, C19, C20, C21, N3, N4, O9, O10, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15a, C16a, C17a, C18a, C19a, C20a, N3a, N4a, O9a, O10a, O6a, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8a, N1a, C6a, C7a, C33, C5a, C2a, O1a, C4a, C9a, C13a, C3a, N2a, C10a, O2a,
 C12a, O4a, O5a, C11a, O3a, C14a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1a)=Sof(H1a)=Sof(O17)=Sof(N6)=Sof(C1b)=Sof(H1b)=Sof(C1c)=Sof(H1ca)=
 Sof(H1cb)=Sof(H)=1-FVAR(1)
 Sof(O14)=Sof(H14d)=Sof(H14e)=Sof(H14a)=Sof(H14b)=Sof(H14a)=Sof(H14b)=FVAR(1)
 Sof(C15a)=Sof(C16a)=Sof(H16a)=Sof(C17a)=Sof(H17a)=Sof(C18a)=Sof(C19a)=
 Sof(H19a)=Sof(C20a)=Sof(C21a)=Sof(H21a)=Sof(N3a)=Sof(O6a)=Sof(N4a)=Sof(O9a)=
 Sof(O10a)=1-FVAR(2)
 Sof(C15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(C19)=Sof(H19)=
 Sof(C20)=Sof(N3)=Sof(O6)=Sof(N4)=Sof(O9)=Sof(O10)=FVAR(2)
 Fixed Sof: C30(0.75) C31(0.75) C32(0.75) N5(0.75) O16(0.75) O35(0.5)
 H35a(0.5) H35b(0.5) C30a(0.25) H30a(0.25) C31a(0.25) H31d(0.25) H31e(0.25)
 H31f(0.25) C32a(0.25) N5a(0.25) O16a(0.25) O19(0.125) H19b(0.125) H19c(0.125)
 O20(0.25) H20a(0.25) H20b(0.25) O18(0.15) H18a(0.15) H18b(0.15) H30(0.75)
 H31a(0.75) H31b(0.75) H31c(0.75) H32a(0.75) H32b(0.75) H32c(0.75) H30a(0.25)
 H32d(0.25) H32e(0.25) H32f(0.25) H31d(0.25) H31e(0.25) H31f(0.25)
7.a Riding coordinates:
 O19(H19b,H19c), O18(H18a,H18b), O20(H20a,H20b), O35(H35a,H35b)
7.b Rotating group:
 O15(H15a,H15b), O14(H14a,H14b)
7.c Ternary CH refined with riding coordinates:
 C1b(H1b)
7.d Me refined with riding coordinates:
 C28(H28a,H28b,H28c), C14a(H14d,H14e,H14c)
7.e Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C19(H19), C23(H23), C24(H24), C25(H25), C1a(H1a),
 C16a(H16a), C17a(H17a), C19a(H19a), C5a(H5a), C3a(H3a), C2a(H2a), C11a(H11a),
 C10a(H10a), C9a(H9a), C7a(H7a), C30(H30), C30a(H30a)
7.f Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C32a(H32d,H32e,H32f), C31a(H31d,
 H31e,H31f)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 372 electrons were 
found in a volume of 1588\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 16[H2O] per Asymmetric Unit 
which account for 320 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;