Crowding out: ligand modifications and their structure directing effects on brucite-like {M<sub>x</sub>(μ<sub>3</sub>-OH)<sub>y</sub>} (M = Co(ii), Ni(ii)) core growth within polymetallic cages.
Slater-Parry, Mari E; Durrant, James P.; Howells, Joshua M.; Pitak, Mateusz B.; Horton, Peter N.; Klooster, Wim T.; Coles, Simon J.; O'Connor, Helen M; Brechin, Euan K.; Barra, Anne-Laure; Jones, Leigh F.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1477–1488; doi:10.1039/c8dt04229b

data_7048400
_publ_section_title
;
 Crowding out: ligand modifications and their structure directing effects
 on brucite-like {M<sub>x</sub>(\m<sub>3</sub>-OH)<sub>y</sub>} (M =
 Co(ii), Ni(ii)) core growth within polymetallic cages.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1477
_journal_page_last               1488
_journal_paper_doi               10.1039/c8dt04229b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C45 H44 N4 O13 Ni2, (C3 H16 O5)'
_chemical_formula_sum            'C48 H60 N4 Ni2 O18'
_chemical_formula_weight         1098.39
_chemical_properties_physical    Moisture-sensitive
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-12-18 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.904(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6966(4)
_cell_length_b                   10.1709(3)
_cell_length_c                   38.0873(11)
_cell_measurement_reflns_used    15137
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.8260
_cell_measurement_theta_min      2.5670
_cell_volume                     4912.1(3)
_computing_cell_refinement       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_data_collection       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_data_reduction        'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_molecular_graphics
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'dtrek-crysalispro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            50784
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.142
_diffrn_source                   'fine-focus sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
crysalispro 1.171.39.9g (rigaku oxford diffraction, 2015)
empirical absorption correction using spherical harmonics,
 implemented in scale3 abspack scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             2008
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.418
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8992
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+9.6538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6615
_reflns_number_total             8992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04229b2.cif
_cod_data_source_block           msp3s
_cod_depositor_comments
'Adding full bibliography for 7048397--7048403.cif.'
_cod_database_code               7048400
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              4681
_shelx_fab_checksum              46301
_platon_squeeze_void_probe_radius 1.20