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_7048397
_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         'C30 H28 N2 Ni O4'
_chemical_formula_sum            'C30 H28 N2 Ni O4'
_chemical_formula_weight         539.25
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-12-12 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                69.232(4)
_cell_angle_beta                 87.650(4)
_cell_angle_gamma                89.471(4)
_cell_formula_units_Z            1
_cell_length_a                   6.7178(3)
_cell_length_b                   9.3940(4)
_cell_length_c                   10.1699(4)
_cell_measurement_reflns_used    6995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4810
_cell_measurement_theta_min      2.3460
_cell_volume                     599.58(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.888
_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   -106.00  74.00   1.00    5.00    --  -16.00   0.00 114.00  180
  2  \w    -70.00  23.00   1.00    5.00    --  -16.00 -72.00-115.00   93
  3  \w    -61.00  23.00   1.00    5.00    --  -16.00 -72.00  81.00   84
  4  \w    -30.00  -2.00   1.00    5.00    --  -16.00  72.00  16.00   28
  5  \w    -63.00 -48.00   1.00    5.00    --  -16.00 -72.00-148.00   15
  6  \w   -106.00  23.00   1.00    5.00    --  -16.00 -72.00  49.00  129
  7  \w    -49.00 -26.00   1.00    5.00    --  -16.00   0.00-148.00   23
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8112
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.681
_diffrn_reflns_theta_min         2.143
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             282
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+0.2447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2929
_reflns_number_total             3018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04229b2.cif
_cod_data_source_block           2016ncs0311
_cod_depositor_comments
'Adding full bibliography for 7048397--7048403.cif.'
_cod_database_code               7048397
_chemical_oxdiff_formula         'C15 H20 N2 O Ni'
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.890
_reflns_odcompleteness_completeness 88.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.62
_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
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              56194
_shelx_shelxl_version_number     2014/7
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.357
_oxdiff_exptl_absorpt_empirical_full_min 0.637