Post-assembly guest oxidation in a metallo-supramolecular host and structural rearrangement to a coordination polymer
Marzio Rancan; Jacopo Tessarolo; Silvio Quicic; Lidia Armelao; Chem.Commun. 50 (2014) 13761–; doi:10.1039/C4cc05422A

data_7115899
_publ_section_title
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 Post-assembly guest oxidation in a metallo-supramolecular host and
 structural rearrangement to a coordination polymer
;
_journal_name_full               Chem.Commun.
_journal_page_first              13761
_journal_paper_doi               10.1039/C4cc05422A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C86 H94 Cu5 N3 O22 P'
_chemical_formula_sum            'C86 H94 Cu5 N3 O22 P'
_chemical_formula_weight         1870.31
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                72.532(3)
_cell_angle_beta                 66.428(3)
_cell_angle_gamma                68.592(4)
_cell_formula_units_Z            2
_cell_length_a                   17.0466(7)
_cell_length_b                   18.6805(7)
_cell_length_c                   21.1943(5)
_cell_measurement_reflns_used    8273
_cell_measurement_temperature    295.9(5)
_cell_measurement_theta_max      25.2280
_cell_measurement_theta_min      2.6060
_cell_volume                     5664.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      295.9(5)
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0279621000
_diffrn_orient_matrix_UB_12      0.0191903000
_diffrn_orient_matrix_UB_13      0.0016904000
_diffrn_orient_matrix_UB_21      -0.0280215000
_diffrn_orient_matrix_UB_22      0.0051516000
_diffrn_orient_matrix_UB_23      0.0345697000
_diffrn_orient_matrix_UB_31      0.0258740000
_diffrn_orient_matrix_UB_32      -0.0363963000
_diffrn_orient_matrix_UB_33      0.0134281000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37372
_diffrn_reflns_theta_full        24.66
_diffrn_reflns_theta_max         24.66
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1934
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         18165
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                12562
_reflns_number_total             18165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05422a2.cif
_cod_data_source_block           exp_506_d085
_cod_original_cell_volume        5664.3(3)
_cod_database_code               7115899
_chemical_oxdiff_formula         'C86 H94 Cu5 N3 O22 P1'
_chemical_oxdiff_usercomment     '13MR04 CHCl3/EtOH'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_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, All O(H,H) groups
2. Restrained distances
 O1W-H1Wa = O1W-H1Wb
 0.9 with sigma of 0.01
 H1Wa-H1Wb
 1.387 with sigma of 0.02
 C48A-C47 \\sim C48B-C47
 with sigma of 0.01
3. Restrained planarity
 C59B, C58B, C57B, C56B, C55A, C54A
 with sigma of 0.1
 C59A, C58A, C57A, C56A, C55B, C54B
 with sigma of 0.1
4. Others
 Sof(C48B)=Sof(H48a)=Sof(H48b)=Sof(H48c)=1-FVAR(1)
 Sof(C48A)=Sof(H48d)=Sof(H48e)=Sof(H48f)=FVAR(1)
 Sof(C59B)=Sof(C54B)=Sof(C58B)=Sof(H58B)=Sof(C56B)=Sof(H56B)=Sof(C57B)=
 Sof(H57B)=Sof(C55B)=Sof(H55B)=1-FVAR(2)
 Sof(C59A)=Sof(C58A)=Sof(H58A)=Sof(C57A)=Sof(H57A)=Sof(C56A)=Sof(H56A)=
 Sof(C55A)=Sof(H55A)=Sof(C54A)=FVAR(2)
5.a Rotating group:
 O1W(H1Wa,H1Wb)
5.b Secondary CH2 refined with riding coordinates:
 C85(H85a,H85b), C86(H86a,H86b), C81(H81a,H81b), C83(H83a,H83b), C82(H82a,
 H82b), C84(H84a,H84b)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C72(H72), C26(H26), C74(H74), C71(H71),
 C23(H23), C73(H73), C40(H40), C58B(H58B), C39(H39), C25(H25), C56B(H56B),
 C41(H41), C42(H42), C24(H24), C57B(H57B), C55B(H55B), C58A(H58A), C57A(H57A),
 C56A(H56A), C55A(H55A)
5.d Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C76(H76a,H76b,H76c), C5(H5a,H5b,H5c), C64(H64a,H64b,
 H64c), C32(H32a,H32b,H32c), C65(H65a,H65b,H65c), C37(H37a,H37b,H37c), C12(H12a,
 H12b,H12c), C53(H53a,H53b,H53c), C80(H80a,H80b,H80c), C1(H1a,H1b,H1c),
 C44(H44a,H44b,H44c), C69(H69a,H69b,H69c), C21(H21a,H21b,H21c), C33(H33a,H33b,
 H33c), C28(H28a,H28b,H28c), C48B(H48a,H48b,H48c), C17(H17a,H17b,H17c),
 C49(H49a,H49b,H49c), C60(H60a,H60b,H60c), C48A(H48d,H48e,H48f)
;