Templated synthesis of Ni(ii) complexes of unsymmetrical Schiff base ligands derived from 1,3-diamino-2-propanol: structural diversity and magnetic properties
Bhunia, Pradip; Maity, Souvik; Mayans, Júlia; Ghosh, Ashutosh; New Journal of Chemistry 46 (2022) 4363–4372; doi:10.1039/D1NJ05638G

data_7061262
_publ_section_title
;
 Templated synthesis of Ni(ii) complexes of unsymmetrical Schiff base
 ligands derived from 1,3-diamino-2-propanol: structural diversity and
 magnetic properties
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4363
_journal_page_last               4372
_journal_paper_doi               10.1039/D1NJ05638G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C56.4 H58.81 N10 Ni6 O16, 23[CH4O]'
_chemical_formula_sum            'C56.4 H58.81 N10 Ni6 O16'
_chemical_formula_weight         1485.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-26 deposited with the CCDC.	2022-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.674(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.199(4)
_cell_length_b                   15.467(2)
_cell_length_c                   17.513(2)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      2.35
_cell_volume                     7529.7(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35077
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.465
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3053
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         12824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0771P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7120
_reflns_number_total             12824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05638g2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'EMPIRICAL' was
changed to 'empirical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7061260--7061262.cif.
;
_cod_original_formula_sum        'C56.40 H58.81 N10 Ni6 O16'
_cod_database_code               7061262
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H58)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
 Sof(H118)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(2)
 Fixed Sof: H84(0.75) H24(0.75) H18(0.25) H78(0.25) C91(0.75) H91A(0.75)
 H91B(0.75) H91C(0.75) C31(0.75) H31A(0.75) H31B(0.75) H31C(0.75) C8(0.25)
 H8A(0.25) H8B(0.25) H8C(0.25) C32(0.25) H32A(0.25) H32B(0.25) H32C(0.25)
 Fixed Uiso: C8(0.1) C32(0.1) C2(0.1) C7(0.1)
3.a Ternary CH refined with riding coordinates:
 C121(H121), C61(H61), C21(H21), C81(H81)
3.b Secondary CH2 refined with riding coordinates:
 N63(H63A,H63B), N123(H12A,H12B), C62(H62A,H62B), C122(H12C,H12D), C22(H22A,
 H22B), C60(H60A,H60B), C120(H12E,H12F), C82(H82A,H82B), C20(H20A,H20B),
 C80(H80A,H80B)
3.c Aromatic/amide H refined with riding coordinates:
 C89(H89), C84(H84), C118(H118), C58(H58), C86(H86), C29(H29), C24(H24),
 C113(H113), C88(H88), C18(H18), C87(H87), C116(H116), C56(H56), C26(H26),
 C53(H53), C115(H115), C54(H54), C28(H28), C27(H27), C55(H55), C73(H73),
 C114(H114), C78(H78), C74(H74), C76(H76), C75(H75), C13(H13), C16(H16),
 C15(H15), C14(H14)
3.d Idealised Me refined as rotating group:
 C91(H91A,H91B,H91C), C31(H31A,H31B,H31C), C8(H8A,H8B,H8C), C32(H32A,H32B,
 H32C), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 408 electrons were 
found in a volume of 2572\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 23[CH4O] per Formula Unit 
which account for 414 electrons per unit cell.
_smtbx_masks_void_probe_radius     1.2
_smtbx_masks_void_truncation_radius  1.2
;
_shelx_res_checksum              28035
_shelx_fab_checksum              68666
_olex2_submission_special_instructions 'No special instructions were received'