Influence of neutral auxiliary ligands on crystal structure and magnetic behaviour of new [MnII2MnIII2] clusters supported by p-adamantylcalix[4]arene
Ovsyannikov, Alexander S.; Strelnikova, Iuliia V.; Samigullina, Aida I.; Islamov, Daut R.; Cherosov, Mikhail A.; Batulin, Ruslan G.; Kiiamov, Airat G.; Gubaidullin, Aidar T.; Dorovatovskii, Pavel V.; Solovieva, Svetlana E.; Antipin, Igor S.; New Journal of Chemistry 48 (2024) 203–215; doi:10.1039/D3NJ04809H

data_7062888
_publ_section_title
;
 Influence of neutral auxiliary ligands on crystal structure and magnetic
 behaviour of new [MnII2MnIII2] clusters supported by
 p-adamantylcalix[4]arene
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              203
_journal_page_last               215
_journal_paper_doi               10.1039/D3NJ04809H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C140 H172 Mn4 N2 O14, C6 H14 N2 O2, H4 O2'
_chemical_formula_sum            'C146 H190 Mn4 N4 O18'
_chemical_formula_weight         2508.77
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-11-15 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.28(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.071(3)
_cell_length_b                   23.504(5)
_cell_length_c                   21.891(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.823
_cell_measurement_theta_min      1.423
_cell_volume                     7196(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79312
_diffrn_reflns_av_R_equivalents  0.1697
_diffrn_reflns_av_unetI/netI     0.1402
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45690
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        27.823
_diffrn_reflns_theta_max         27.823
_diffrn_reflns_theta_min         1.423
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsh, 2010)'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       needle
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.117
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12198
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1987
_refine_ls_R_factor_gt           0.1091
_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^)+(0.1783P)^2^+1.4832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2776
_refine_ls_wR_factor_ref         0.3385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5636
_reflns_number_total             12198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04809h2.cif
_cod_data_source_block           kmv180-1
_cod_depositor_comments
'Adding full bibliography for 7062886--7062889.cif.'
_cod_database_code               7062888
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Shared sites
{H31D, H31A}
{H32D, H32A}
2. Others
 Fixed Sof: C29(0.5) C31B(0.5) H31A(0.5) H31B(0.5) C30B(0.5) H30A(0.5)
 H30B(0.5) C32B(0.5) H32A(0.5) H32B(0.5) C31A(0.5) H31C(0.5) H31D(0.5)
 C32A(0.5) H32C(0.5) H32D(0.5) C30A(0.5) H30C(0.5) H30D(0.5) C59(0.5) C63B(0.5)
 H63B(0.5) C67B(0.5) H67B(0.5) C60B(0.5) H60A(0.5) H60B(0.5) C61B(0.5)
 H61A(0.5) H61B(0.5) C62B(0.5) H62A(0.5) H62B(0.5) C61A(0.5) H61C(0.5)
 H61D(0.5) C62A(0.5) H62C(0.5) H62D(0.5) C60A(0.5) H60C(0.5) H60D(0.5)
 C67A(0.5) H67A(0.5) C65B(0.5) H65B(0.5) C63A(0.5) H63A(0.5) C65A(0.5)
 H65A(0.5) C68A(0.5) H68A(0.5) H68B(0.5) C64A(0.5) H64A(0.5) H64B(0.5)
 C64B(0.5) H64C(0.5) H64D(0.5) C68B(0.5) H68C(0.5) H68D(0.5) C66B(0.5)
 H66A(0.5) H66B(0.5) C66A(0.5) H66C(0.5) H66D(0.5) C33A(0.5) H33A(0.5)
 C35A(0.5) H35A(0.5) C37B(0.5) H37B(0.5) C37A(0.5) H37A(0.5) C35B(0.5)
 H35B(0.5) C33B(0.5) H33B(0.5) C34B(0.5) H34A(0.5) H34B(0.5) C38B(0.5)
 H38A(0.5) H38B(0.5) C38A(0.5) H38C(0.5) H38D(0.5) C34A(0.5) H34C(0.5)
 H34D(0.5) C36B(0.5) H36A(0.5) H36B(0.5) C36A(0.5) H36C(0.5) H36D(0.5)
 Fixed Uiso: H5A(0.048) H3(0.049) H26(0.05) H6A(0.156) H6B(0.156) H24(0.049)
 H17(0.045) H22A(0.047) H22B(0.047) H8A(0.046) H8B(0.046) H19(0.046) H12(0.056)
 H15A(0.052) H15B(0.052) H1A(0.048) H1B(0.048) H10(0.053) H42A(0.063)
 H42B(0.063) H40A(0.07) H40B(0.07) H74A(0.093) H74B(0.093) H74C(0.093)
 H57(0.095) H73(0.085) H75A(0.097) H75B(0.097) H75C(0.097) H44A(0.105)
 H44B(0.105) H43(0.081) H45(0.096) H41A(0.083) H41B(0.083) H53(0.095)
 H47(0.078) H52A(0.095) H52B(0.095) H54A(0.095) H54B(0.095) H58A(0.095)
 H58B(0.095) H50A(0.095) H50B(0.095) H51A(0.095) H51B(0.095) H48A(0.087)
 H48B(0.087) H46A(0.101) H46B(0.101) H70(0.11) H72A(0.196) H72B(0.196)
 H72C(0.196) H55(0.095) H56A(0.095) H56B(0.095) H31A(0.063) H31B(0.063)
 H71A(0.204) H71B(0.204) H71C(0.204) H30A(0.063) H30B(0.063) H32A(0.063)
 H32B(0.063) H31C(0.063) H31D(0.063) H32C(0.063) H32D(0.063) H30C(0.063)
 H30D(0.063) H63B(0.05) H67B(0.05) H60A(0.05) H60B(0.05) H61A(0.05) H61B(0.05)
 H62A(0.05) H62B(0.05) H61C(0.05) H61D(0.05) H62C(0.05) H62D(0.05) H60C(0.05)
 H60D(0.05) H67A(0.05) H65B(0.05) H63A(0.05) H65A(0.05) H68A(0.05) H68B(0.05)
 H64A(0.05) H64B(0.05) H64C(0.05) H64D(0.05) H68C(0.05) H68D(0.05) H66A(0.05)
 H66B(0.05) H66C(0.05) H66D(0.05) H33A(0.063) H35A(0.063) H37B(0.063)
 H37A(0.063) H35B(0.063) H33B(0.063) H34A(0.063) H34B(0.063) H38A(0.063)
 H38B(0.063) H38C(0.063) H38D(0.063) H34C(0.063) H34D(0.063) H36A(0.063)
 H36B(0.063) H36C(0.063) H36D(0.063) H7A(0.136) H7B(0.136)
 Fixed X: H5A(0.713885) H3(0.466406) H26(0.271158) H6A(0.798834) H6B(0.736803)
 H24(0.112266) H17(0.43412) H22A(0.219722) H22B(0.142143) H8A(0.778396)
 H8B(0.702665) H19(0.193002) H12(0.630235) H15A(0.520083) H15B(0.534746)
 H1A(0.38895) H1B(0.408032) H10(0.791221) H42A(0.670408) H42B(0.743576)
 H40A(0.792493) H40B(0.70072) H74A(0.435558) H74B(0.492134) H74C(0.539331)
 H57(0.13313) H73(0.530403) H75A(0.300633) H75B(0.326311) H75C(0.3635)
 H44A(0.968338) H44B(0.954415) H43(0.820147) H45(1.009971) H41A(0.888161)
 H41B(0.907147) H53(0.407885) H47(0.77096) H52A(0.151974) H52B(0.237427)
 H54A(0.308942) H54B(0.372316) H58A(0.292727) H58B(0.25555) H50A(0.42527)
 H50B(0.396571) H51A(0.30051) H51B(0.191483) H48A(0.825981) H48B(0.720853)
 H46A(0.903939) H46B(0.937831) H70(0.639837) H72A(0.68121) H72B(0.77166)
 H72C(0.785096) H55(0.210615) H56A(0.094943) H56B(0.131663) H31A(0.70193)
 H31B(0.758512) H71A(0.865187) H71B(0.911009) H71C(0.859337) H30A(0.671709)
 H30B(0.56012) H32A(0.473904) H32B(0.531669) H31C(0.591044) H31D(0.700908)
 H32C(0.502387) H32D(0.47247) H30C(0.75081) H30D(0.671554) H63B(0.103094)
 H67B(0.036269) H60A(0.210996) H60B(0.147474) H61A(-0.012315) H61B(0.010773)
 H62A(0.084571) H62B(0.169959) H61C(0.129047) H61D(0.037389) H62C(0.043333)
 H62D(-0.011103) H60C(0.222317) H60D(0.191937) H67A(-0.10576) H65B(-0.122951)
 H63A(0.132963) H65A(-0.012757) H68A(-0.02057) H68B(0.044312) H64A(0.124669)
 H64B(0.028545) H64C(-0.072223) H64D(-0.022927) H68C(0.02056) H68D(0.130562)
 H66A(-0.103062) H66B(-0.089919) H66C(-0.10292) H66D(-0.118315) H33A(0.765615)
 H35A(0.681375) H37B(0.506796) H37A(0.482411) H35B(0.792233) H33B(0.65305)
 H34A(0.760138) H34B(0.795142) H38A(0.580549) H38B(0.504823) H38C(0.595936)
 H38D(0.63055) H34C(0.76079) H34D(0.796815) H36A(0.666825) H36B(0.646567)
 H36C(0.525556) H36D(0.592636) H7A(0.486023) H7B(0.493403)
 Fixed Y: H5A(0.425831) H3(0.486255) H26(0.503319) H6A(0.454132) H6B(0.423157)
 H24(0.408883) H17(0.252633) H22A(0.458502) H22B(0.414988) H8A(0.470206)
 H8B(0.498193) H19(0.319208) H12(0.266915) H15A(0.37883) H15B(0.311238)
 H1A(0.566578) H1B(0.57387) H10(0.365939) H42A(0.193767) H42B(0.198947)
 H40A(0.288922) H40B(0.248511) H74A(0.147105) H74B(0.110212) H74C(0.166791)
 H57(0.158957) H73(0.243067) H75A(0.154671) H75B(0.184926) H75C(0.121786)
 H44A(0.179318) H44B(0.24705) H43(0.202114) H45(0.217399) H41A(0.262035)
 H41B(0.2978) H53(0.111371) H47(0.113358) H52A(0.236267) H52B(0.238115)
 H54A(0.055585) H54B(0.094111) H58A(0.14677) H58B(0.088015) H50A(0.185443)
 H50B(0.21172) H51A(0.181339) H51B(0.197479) H48A(0.115236) H48B(0.142311)
 H46A(0.158702) H46B(0.124591) H70(0.630349) H72A(0.728266) H72B(0.741012)
 H72C(0.735261) H55(0.089888) H56A(0.140646) H56B(0.084053) H31A(0.482658)
 H31B(0.433437) H71A(0.607802) H71B(0.663462) H71C(0.667572) H30A(0.3486)
 H30B(0.34135) H32A(0.417289) H32B(0.472193) H31C(0.489631) H31D(0.480908)
 H32C(0.360614) H32D(0.417969) H30C(0.391874) H30D(0.345173) H63B(0.453799)
 H67B(0.308414) H60A(0.445423) H60B(0.50166) H61A(0.44561) H61B(0.501709)
 H62A(0.356583) H62B(0.35775) H61C(0.520338) H61D(0.516298) H62C(0.368506)
 H62D(0.426895) H60C(0.429456) H60D(0.37038) H67A(0.370239) H65B(0.453418)
 H63A(0.371997) H65A(0.520056) H68A(0.345858) H68B(0.326087) H64A(0.472243)
 H64B(0.443534) H64C(0.456213) H64D(0.508361) H68C(0.365567) H68D(0.358269)
 H66A(0.364035) H66B(0.357232) H66C(0.472304) H66D(0.44521) H33A(0.314447)
 H35A(0.461262) H37B(0.408018) H37A(0.343081) H35B(0.429474) H33B(0.281497)
 H34A(0.330485) H34B(0.343808) H38A(0.315314) H38B(0.321676) H38C(0.284274)
 H38D(0.293647) H34C(0.37262) H34D(0.410647) H36A(0.394901) H36B(0.458385)
 H36C(0.429566) H36D(0.381775) H7A(0.667818) H7B(0.609758)
 Fixed Z: H5A(0.818558) H3(0.868685) H26(0.836267) H6A(0.52933) H6B(0.477301)
 H24(0.707197) H17(0.582769) H22A(0.580283) H22B(0.60153) H8A(0.727196)
 H8B(0.675611) H19(0.636599) H12(0.611414) H15A(0.520583) H15B(0.522097)
 H1A(0.809349) H1B(0.739007) H10(0.732349) H42A(0.683803) H42B(0.633013)
 H40A(0.795113) H40B(0.783399) H74A(0.19713) H74B(0.250796) H74C(0.226827)
 H57(0.729096) H73(0.287754) H75A(0.266369) H75B(0.331578) H75C(0.320634)
 H44A(0.814665) H44B(0.81469) H43(0.849238) H45(0.718349) H41A(0.651223)
 H41B(0.713502) H53(0.714406) H47(0.687926) H52A(0.662741) H52B(0.717246)
 H54A(0.651525) H54B(0.611618) H58A(0.769532) H58B(0.738666) H50A(0.642816)
 H50B(0.705845) H51A(0.550653) H51B(0.557535) H48A(0.793094) H48B(0.781929)
 H46A(0.650576) H46B(0.71253) H70(0.585752) H72A(0.579222) H72B(0.542955)
 H72C(0.616236) H55(0.56437) H56A(0.621098) H56B(0.656813) H31A(0.953337)
 H31B(0.922055) H71A(0.543488) H71B(0.576974) H71C(0.508262) H30A(0.877959)
 H30B(0.884482) H32A(0.937719) H32B(0.96439) H31C(0.96793) H31D(0.957786)
 H32C(0.903065) H32D(0.935432) H30C(0.905111) H30D(0.883552) H63B(0.981449)
 H67B(0.878837) H60A(0.905585) H60B(0.893452) H61A(0.767802) H61B(0.808254)
 H62A(0.792102) H62B(0.846488) H61C(0.866096) H61D(0.815681) H62C(0.784336)
 H62D(0.766663) H60C(0.896504) H60D(0.862867) H67A(0.831556) H65B(0.840118)
 H63A(0.962082) H65A(0.918599) H68A(0.929929) H68B(0.878271) H64A(0.966829)
 H64B(0.985104) H64C(0.948851) H64D(0.916357) H68C(0.971475) H68D(0.960025)
 H66A(0.893429) H66B(0.821934) H66C(0.837194) H66D(0.902189) H33A(0.977237)
 H35A(1.063584) H37B(1.047814) H37A(1.008942) H35B(1.032237) H33B(0.959902)
 H34A(1.039692) H34B(0.973962) H38A(1.047693) H38B(0.987908) H38C(0.964243)
 H38D(1.036008) H34C(1.065544) H34D(1.01204) H36A(1.088596) H36B(1.064389)
 H36C(1.051619) H36D(1.086022) H7A(0.649962) H7B(0.656872)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27460
_shelx_hkl_checksum              48164
_shelx_fab_checksum              34953
_olex2_submission_special_instructions 'No special instructions were received'