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_7041065
_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         'C10 H24 Mn N3 O7, N O3'
_chemical_formula_sum            'C10 H24 Mn N4 O10'
_chemical_formula_weight         415.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-24
_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            8
_cell_length_a                   13.4000(2)
_cell_length_b                   13.8810(2)
_cell_length_c                   17.5344(3)
_cell_measurement_reflns_used    4178
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.000
_cell_volume                     3261.49(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       COLLECT
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  kappaCCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0120
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7038
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'fine focus sealed tube'
_diffrn_source_type              'Nonius FR590 Sealed Tube Generator'
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  0.4300
_exptl_absorpt_correction_T_min  0.2498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0384 before and 0.0294 after correction.
The Ratio of minimum to maximum transmission is 0.5809.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       needle
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3731
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+1.8497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3196
_reflns_number_total             3731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03914f2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 7041065--7041066.cif.'
_cod_database_code               7041065
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 O2-H2
 0.85 with sigma of 0.01
 O3-H3
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 C4-H1
 1.900568 with sigma of 0.02
 Mn1-H1
 2.899882 with sigma of 0.02
 C6-H2
 1.905844 with sigma of 0.02
 Mn1-H2
 2.986539 with sigma of 0.02
 C8-H3
 1.898748 with sigma of 0.02
 Mn1-H3
 2.92269 with sigma of 0.02
 C10-H4
 1.896074 with sigma of 0.02
 Mn1-H4
 2.894578 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
;
_shelx_res_checksum              3490
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'