Core expansion of bis-calix[4]arene-supported clusters.
Coletta, Marco; McLellan, Ross; Waddington, Amy; Sanz, Sergio; Gagnon, Kevin J.; Teat, Simon J.; Brechin, Euan K.; Dalgarno, Scott J.; Chemical communications (Cambridge, England) 52 (2016) 14246–14249; doi:10.1039/c6cc08059f

data_7125261
_publ_section_title
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 Core expansion of bis-calix[4]arene-supported clusters.
;
_journal_issue                   99
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14246
_journal_page_last               14249
_journal_paper_doi               10.1039/c6cc08059f
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C206 H278 Gd2 Mn8 N8 O36, 2(N O3), 2(O)'
_chemical_formula_sum            'C206 H280 Gd2 Mn8 N10 O44'
_chemical_formula_weight         4354.40
_chemical_name_common            Mn8Gd2
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-09 deposited with the CCDC.
2016-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.149(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.0960(7)
_cell_length_b                   19.1570(6)
_cell_length_c                   27.0764(9)
_cell_measurement_temperature    100(2)
_cell_volume                     11063.0(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            136715
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.886
_diffrn_reflns_theta_min         1.900
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1345 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.9216.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       plate
_exptl_crystal_F_000             4532
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.638
_refine_diff_density_min         -1.980
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         24604
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0834
_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^)+(0.1551P)^2^+28.0563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2489
_refine_ls_wR_factor_ref         0.2740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18689
_reflns_number_total             24604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08059f4.cif
_cod_data_source_block           aw20h
_cod_database_code               7125261
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.608
_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. Restrained distances
 C78A-C77 = C78-C77 = C80A-C77 = C80-C77 = C79A-C77 = C79-C77
 1.54 with sigma of 0.02
 O10-C92 = O10-C92A
 1.2 with sigma of 0.02
 N2-C92 = N2-C92A = N2-C94 = N2-C94A = N2-C93 = N2-C93A
 1.45 with sigma of 0.02
 C34A-C33 = C34-C33 = C36A-C33 = C36-C33 = C35A-C33 = C35-C33
 1.54 with sigma of 0.02
 N2-C93A = N2-C93 = N2-C94A = N2-C94 = N2-C92A = N2-C92 = N4-C97 = N4-C96 = N4-
 C95 = N1-C89 = N1-C91 = N1-C90 = N3-C98 = N3-C100 = N3-C99
 1.45 with sigma of 0.02
 O10-C92 = O10-C92A = O11-C95 = O9-C89 = O12-C98
 1.2 with sigma of 0.02
 O15-C101
 1.2 with sigma of 0.02
 O15-C101
 1.2 with sigma of 0.02
 C78A-C80A
 2.54 with sigma of 0.04
 C80A-C79A
 2.54 with sigma of 0.04
 C79A-C78A
 2.54 with sigma of 0.04
 C78-C80
 2.54 with sigma of 0.04
 C80-C79
 2.54 with sigma of 0.04
 C79-C78
 2.54 with sigma of 0.04
 C34A-C36A
 2.54 with sigma of 0.04
 C36A-C35A
 2.54 with sigma of 0.04
 C35A-C34A
 2.54 with sigma of 0.04
 C34-C36
 2.54 with sigma of 0.04
 C36-C35
 2.54 with sigma of 0.04
 C35-C34
 2.54 with sigma of 0.04
 O1AA-O0AA
 2.54 with sigma of 0.04
 O0AA-O3AA
 2.54 with sigma of 0.04
 O3AA-O1AA
 2.54 with sigma of 0.04
 N0AA-O3AA \\sim N0AA-O0AA \\sim N0AA-O1AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Gd1 \\sim Mn3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Gd1A \\sim Mn3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C98) = Uanis(N3) = Uanis(C100) = Uanis(C99) = Uanis(O12)
Uanis(C102) = Uanis(O16)
Uanis(O9) = Uanis(C89) = Uanis(N1) = Uanis(C90) = Uanis(C91)
Uanis(O3AA) = Uanis(O0AA) = Uanis(N0AA) = Uanis(O1AA)
Uanis(C78A) = Uanis(C78) = Uanis(C80A) = Uanis(C80) = Uanis(C79A) = Uanis(C79)
Uanis(C92A) = Uanis(C92) = Uanis(C94) = Uanis(C94A) = Uanis(C93) = Uanis(C93A)
Uanis(C34A) = Uanis(C34) = Uanis(C36A) = Uanis(C36) = Uanis(C35A) = Uanis(C35)
4. Others
 Fixed Sof: Gd1(0.7) Gd1A(0.3) O13(0.7) C92(0.65) H92(0.65) C35(0.75)
 H35A(0.75) H35B(0.75) H35C(0.75) C78(0.7) H78A(0.7) H78B(0.7) H78C(0.7)
 C79(0.7) H79A(0.7) H79B(0.7) H79C(0.7) C94(0.65) H94A(0.65) H94B(0.65)
 H94C(0.65) C80(0.7) H80A(0.7) H80B(0.7) H80C(0.7) C34(0.75) H34A(0.75)
 H34B(0.75) H34C(0.75) C93(0.65) H93A(0.65) H93B(0.65) H93C(0.65) C36(0.75)
 H36A(0.75) H36B(0.75) H36C(0.75) C104(0.7) H10A(0.7) H10B(0.7) H10C(0.7)
 Mn3(0.7) C103(0.3) H10J(0.3) H10K(0.3) H10L(0.3) O13A(0.3) Mn3A(0.3) O4AA(0.5)
 O2AA(0.5) C92A(0.35) H92A(0.35) C93A(0.35) H93D(0.35) H93E(0.35) H93F(0.35)
 C94A(0.35) H94D(0.35) H94E(0.35) H94F(0.35) C80A(0.3) H80D(0.3) H80E(0.3)
 H80F(0.3) C79A(0.3) H79D(0.3) H79E(0.3) H79F(0.3) C78A(0.3) H78D(0.3)
 H78E(0.3) H78F(0.3) C34A(0.25) H34D(0.25) H34E(0.25) H34F(0.25) C35A(0.25)
 H35D(0.25) H35E(0.25) H35F(0.25) C36A(0.25) H36D(0.25) H36E(0.25) H36F(0.25)
5.a Ternary CH refined with riding coordinates:
 C45(H45), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B), C59(H59A,H59B), C52(H52A,H52B), C7(H7A,H7B), C21(H21A,H21B),
 C14(H14A,H14B)
5.c Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C94(H94A,H94B,
 H94C), C80(H80A,H80B,H80C), C34(H34A,H34B,H34C), C93(H93A,H93B,H93C), C36(H36A,
 H36B,H36C), C93A(H93D,H93E,H93F), C94A(H94D,H94E,H94F), C80A(H80D,H80E,H80F),
 C79A(H79D,H79E,H79F), C78A(H78D,H78E,H78F), C34A(H34D,H34E,H34F), C35A(H35D,
 H35E,H35F), C36A(H36D,H36E,H36F)
5.d Aromatic/amide H refined with riding coordinates:
 C68(H68), C61(H61), C47(H47), C70(H70), C63(H63), C49(H49), C25(H25),
 C56(H56), C2(H2), C95(H95), C23(H23), C4(H4), C54(H54), C16(H16), C9(H9),
 C18(H18), C11(H11), C92(H92), C89(H89), C98(H98), C92A(H92A)
5.e Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C84(H84A,H84B,
 H84C), C75(H75A,H75B,H75C), C74(H74A,H74B,H74C), C82(H82A,H82B,H82C), C96(H96A,
 H96B,H96C), C97(H97A,H97B,H97C), C86(H86A,H86B,H86C), C76(H76A,H76B,H76C),
 C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C90(H90A,H90B,H90C), C91(H91A,
 H91B,H91C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C104(H10A,H10B,H10C), C102(H10D,H10E,H10F), C99(H99A,H99B,H99C), C100(H10G,
 H10H,H10I), C103(H10J,H10K,H10L), C101(H10M,H10N,H10O)
;
_shelx_res_checksum              49315
_olex2_submission_special_instructions 'No special instructions were received'