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_7048401
_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         'C60 H62 Br4 N6 Ni4 O16), C2 H3 N'
_chemical_formula_sum            'C62 H65 Br4 N7 Ni4 O16'
_chemical_formula_weight         1718.69
_chemical_name_common            '[Ni4-Br]'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-12-12 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                105.986(2)
_cell_angle_beta                 90.324(3)
_cell_angle_gamma                105.805(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1808(5)
_cell_length_b                   15.8405(5)
_cell_length_c                   20.5877(5)
_cell_measurement_reflns_used    17423
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.4570
_cell_measurement_theta_min      2.1820
_cell_volume                     3359.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35525
_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         25.350
_diffrn_reflns_theta_min         1.900
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63645
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1732
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.247
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         12305
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1221P)^2^+4.8871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9906
_reflns_number_total             12305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04229b2.cif
_cod_data_source_block           ni4-br-
_cod_depositor_comments
'Adding full bibliography for 7048397--7048403.cif.'
_cod_database_code               7048401
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.600
_shelx_estimated_absorpt_t_max   0.871
_shelx_res_checksum              50623