Rational serendipity: "undirected" synthesis of a large {MnCu} complex from pre-formed Mn(II) building blocks.
Frost, Jamie M.; Kettles, Fraser J.; Wilson, Claire; Murrie, Mark; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18094–18097; doi:10.1039/c6dt03914f

data_7041066
_publ_section_title
;
 Rational serendipity: &quot;undirected&quot; synthesis of a large {MnCu}
 complex from pre-formed Mn(II) building blocks.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18094
_journal_page_last               18097
_journal_paper_doi               10.1039/c6dt03914f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C96 H128 Cu5 Mn10 N8 O44, 4(N O3), 4(C H4 O)'
_chemical_formula_sum            'C100 H144 Cu5 Mn10 N12 O60'
_chemical_formula_weight         3341.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-29 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5814(6)
_cell_length_b                   27.5814(6)
_cell_length_c                   18.4546(4)
_cell_measurement_reflns_used    6445
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      2.000
_cell_volume                     14039.0(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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    Superflip
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            6405
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.371
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         2.442
_diffrn_source                   'fine focus sealed tube'
_diffrn_source_type              'Nonius FR590 Sealed Tube Generator'
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_T_max  0.4282
_exptl_absorpt_correction_T_min  0.1213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0484 before and 0.0336 after correction.
The Ratio of minimum to maximum transmission is 0.2833.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             6812
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.872
_refine_diff_density_min         -2.519
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6405
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0707P)^2^+64.8638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5223
_reflns_number_total             6405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03914f2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7041065--7041066.cif.'
_cod_original_cell_volume        14039.0(7)
_cod_database_code               7041066
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9B = O9-H9A
 0.85 with sigma of 0.02
 O1M-C2M
 1.41 with sigma of 0.02
 O41-C10 = O40-C10 = O42-C10
 1.41 with sigma of 0.02
 O1M-C2M
 1.41 with sigma of 0.02
 N3-O13 \\sim N3-O14 \\sim N3-O15 \\sim N3-O12 \\sim N3-O17
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C2M
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O13)=Sof(O14)=1-FVAR(1)
 Sof(O15)=Sof(O17)=FVAR(1)
 Fixed Sof: O40(0.3) H40(0.3) O41(0.3) H41(0.3) O42(0.4) H42(0.4) H10B(0.4)
 H10A(0.4) H10F(0.3) H10E(0.3) H10C(0.3) H10D(0.3)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9C,H9D), C10(H10B,H10A), C10(H10F,H10E), C10(H10C,H10D)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24)
5.c Tetrahedral OH refined with riding coordinates:
 O40(H40), O41(H41), O42(H42)
5.d Idealised Me refined as rotating group:
 C2M(H2MA,H2MB,H2MC)
5.e Idealised tetrahedral OH refined as rotating group:
 O1M(H1M)
;
_shelx_res_checksum              24997
_shelx_fab_checksum              22788
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'