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_7125260
_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
'C199.2 H260.8 Mn10 N6.4 O34.4, 5.6(C3 H7 N O)'
_chemical_formula_sum            'C216 H310 Mn10 N12 O40'
_chemical_formula_weight         4264.14
_chemical_name_common            Mn10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                69.512(2)
_cell_angle_beta                 75.796(2)
_cell_angle_gamma                81.501(2)
_cell_formula_units_Z            1
_cell_length_a                   14.9101(5)
_cell_length_b                   17.9438(5)
_cell_length_c                   22.3792(7)
_cell_measurement_temperature    100(2)
_cell_volume                     5424.6(3)
_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 0.677
_diffrn_measured_fraction_theta_max 0.997
_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  0.0696
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.677
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54412
_diffrn_reflns_point_group_measured_fraction_full 0.677
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         24.126
_diffrn_reflns_theta_min         2.137
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0958 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.8795.
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    1.305
_exptl_crystal_description       plate
_exptl_crystal_F_000             2260
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.233
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         13284
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0762
_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^)+(0.1199P)^2^+23.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9258
_reflns_number_total             13284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08059f4.cif
_cod_data_source_block           mc102e3
_cod_database_code               7125260
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.924
_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
 C41-C42A = C42-C41 = C43-C41 = C43A-C41 = C41-C44
 1.54 with sigma of 0.02
 C41-C42A = C42-C41 = C44A-C41 = C41-C44 = C43A-C41 = C43-C41
 1.54 with sigma of 0.02
 O17-C105 = N1-C101 = N1-C102 = N1-C103 = N13-C91 = N13-C90 = N13-C89
 1.45 with sigma of 0.02
 O03D-C101 = O9-C89
 1.2 with sigma of 0.02
 O17-C105
 1.2 with sigma of 0.02
 O16-C104
 1.2 with sigma of 0.02
 O03I-C03S
 1.2 with sigma of 0.02
 N001-C0BA = N001-C006 = N001-C004 = N03H-C03S = N03H-C03O = N03H-C03Q
 1.45 with sigma of 0.02
 N2-C92A = N2-C92 = N2-C94A = N2-C94 = N2-C93A = N2-C93
 1.45 with sigma of 0.02
 C42A-C44A
 2.54 with sigma of 0.04
 C44A-C43
 2.54 with sigma of 0.04
 C43-C42
 2.54 with sigma of 0.04
 C42A-C44A
 2.54 with sigma of 0.04
 C44A-C43A
 2.54 with sigma of 0.04
 C43A-C42A
 2.54 with sigma of 0.04
 C42A-C44
 2.54 with sigma of 0.04
 C44-C43
 2.54 with sigma of 0.04
 C43-C42
 2.54 with sigma of 0.04
 C92-C93 \\sim C93-C94 \\sim C94-C92 \\sim C92A-C93A \\sim C93A-C94A \\sim
C94A-C92A
 with sigma of 0.02
 C89-C90 \\sim C90-C91 \\sim C91-C89
 with sigma of 0.02
 N4-O12 \\sim N3-O11 \\sim N001-O003
 with sigma of 0.02
 C0BA-C004 \\sim C004-C006 \\sim C006-C0BA
 with sigma of 0.02
 C92-C93 \\sim C93-C94 \\sim C94-C92 \\sim C92A-C93A \\sim C93A-C94A \\sim
C94A-C92A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41) = Uanis(C42) = Uanis(C44) = Uanis(C43)
Uanis(C92) = Uanis(C92A) = Uanis(N2) = Uanis(C93) = Uanis(C93A) = Uanis(C94) =
Uanis(C94A)
Uanis(C006) = Uanis(N001) = Uanis(C004) = Uanis(C0BA) = Uanis(O003)
Uanis(N03H) = Uanis(C03S) = Uanis(O03I) = Uanis(C03O) = Uanis(C03Q)
Uanis(C105) = Uanis(O17)
Uanis(C42A) = Uanis(C42) = Uanis(C44A) = Uanis(C44) = Uanis(C43A) = Uanis(C43)
Uanis(O9) = Uanis(C89) = Uanis(N13) = Uanis(C91) = Uanis(C102) = Uanis(N1) =
Uanis(C101) = Uanis(C90) = Uanis(O03D) = Uanis(C103)
4. Others
 Fixed Sof: N1(0.8) C92(0.85) H92(0.85) C42(0.6) H42A(0.6) H42B(0.6) H42C(0.6)
 C44(0.6) H44A(0.6) H44B(0.6) H44C(0.6) C93(0.85) H93A(0.85) H93B(0.85)
 H93C(0.85) O03D(0.8) C94(0.85) H94A(0.85) H94B(0.85) H94C(0.85) C43(0.6)
 H43A(0.6) H43B(0.6) H43C(0.6) C102(0.8) H10J(0.8) H10K(0.8) H10L(0.8)
 C101(0.8) H101(0.8) O9(0.2) C92A(0.15) H92A(0.15) C93A(0.15) H93D(0.15)
 H93E(0.15) H93F(0.15) C94A(0.15) H94D(0.15) H94E(0.15) H94F(0.15) C103(0.8)
 H10M(0.8) H10N(0.8) H10O(0.8) C89(0.2) H89(0.2) N13(0.2) C90(0.2) H90A(0.2)
 H90B(0.2) H90C(0.2) C91(0.2) H91A(0.2) H91B(0.2) H91C(0.2) C42A(0.4) H42D(0.4)
 H42E(0.4) H42F(0.4) C43A(0.4) H43D(0.4) H43E(0.4) H43F(0.4) C44A(0.4)
 H44D(0.4) H44E(0.4) H44F(0.4)
5.a Ternary CH refined with riding coordinates:
 C28(H28), C45(H45)
5.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B), C21(H21A,H21B), C52(H52A,H52B), C7(H7A,H7B), C59(H59A,H59B),
 C14(H14A,H14B)
5.c Me refined with riding coordinates:
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C97(H97A,H97B,H97C), C93(H93A,H93B,
 H93C), C96(H96A,H96B,H96C), C104(H10D,H10E,H10F), C94(H94A,H94B,H94C),
 C43(H43A,H43B,H43C), C102(H10J,H10K,H10L), C105(H10G,H10H,H10I), C03O(H03A,
 H03B,H03C), C03Q(H03D,H03E,H03F), C004(H00A,H00B,H00C), C006(H00D,H00E,H00F),
 C93A(H93D,H93E,H93F), C94A(H94D,H94E,H94F), C103(H10M,H10N,H10O), C90(H90A,
 H90B,H90C), C91(H91A,H91B,H91C), C42A(H42D,H42E,H42F), C43A(H43D,H43E,H43F),
 C44A(H44D,H44E,H44F)
5.d Aromatic/amide H refined with riding coordinates:
 C47(H47), C70(H70), C68(H68), C2(H2), C61(H61), C63(H63), C49(H49), C4(H4),
 C23(H23), C18(H18), C25(H25), C54(H54), C16(H16), C56(H56), C9(H9), C11(H11),
 C98(H98), C95(H95), C92(H92), C101(H101), C03S(H03S), C92A(H92A), C89(H89),
 C0BA(H0BA)
5.e Idealised Me refined as rotating group:
 C86(H86A,H86B,H86C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C88(H88A,H88B,
 H88C), C79(H79A,H79B,H79C), C34(H34A,H34B,H34C), C78(H78A,H78B,H78C), C40(H40A,
 H40B,H40C), C38(H38A,H38B,H38C), C75(H75A,H75B,H75C), C32(H32A,H32B,H32C),
 C87(H87A,H87B,H87C), C82(H82A,H82B,H82C), C100(H10A,H10B,H10C), C74(H74A,H74B,
 H74C), C99(H99A,H99B,H99C), C76(H76A,H76B,H76C), C30(H30A,H30B,H30C), C80(H80A,
 H80B,H80C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C)
;
_shelx_res_checksum              43933
_olex2_submission_special_instructions 'No special instructions were received'