Evolution of Manganese-Calcium Cluster Structures based on Nitrogen and Oxygen Donor Ligands
Benniston, A. C.; Melnic, Silvia; Waddell, Paul G.; Sova, Sergiu; CrystEngComm  (2017) –; doi:10.1039/C7CE00931C

data_7228513
_publ_section_title
;
 Evolution of Manganese-Calcium Cluster Structures based on Nitrogen and
 Oxygen Donor Ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00931C
_journal_year                    2017
_chemical_formula_moiety         '2(C78 H78 Ca2 Mn6 N6 O27), 8(Cl O4), 13(H2 O)'
_chemical_formula_sum            'C156 H182 Ca4 Cl8 Mn12 N12 O99'
_chemical_formula_weight         4912.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-05-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.2590(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.8236(3)
_cell_length_b                   14.88011(20)
_cell_length_c                   27.1462(4)
_cell_measurement_reflns_used    9505
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      65.7480
_cell_measurement_theta_min      3.3750
_cell_volume                     9961.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   30.00  108.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4655   38.0000 -120.0000 78

  2 omega   19.00  114.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4655   38.0000  -30.0000 95

  3 omega   16.00   41.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -30.0000 25

  4 omega   24.00   96.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   30.0000 72

  5 omega    9.00   35.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000   60.0000 26

  6 omega   70.00   95.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  150.0000 25

  7 omega   31.00   77.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 46

  8 omega   40.00   84.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  -60.0000 44

  9 omega   13.00   66.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000   90.0000 53

 10 omega   15.00   81.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -60.0000 66

 11 omega   86.00  155.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   86.0000  -15.0000 69

 12 omega   20.00   56.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  150.0000 36

 13 omega   53.00  114.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  120.0000 61

 14 omega   18.00   69.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  120.0000 51

 15 omega   16.00   67.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  150.0000 51

 16 omega   85.00  125.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000 -150.0000 40

 17 omega  140.00  166.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -60.0000 26

 18 omega   19.00   69.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -90.0000 50

 19 omega -115.00  -12.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4655  -57.0000   90.0000 103

 20 omega -102.00  -22.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4655  131.0000 -130.0000 80

 21 omega   12.00  115.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4655   57.0000   30.0000 103

 22 omega   63.00  114.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000  -90.0000 51
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0127921000
_diffrn_orient_matrix_UB_12      -0.0239640000
_diffrn_orient_matrix_UB_13      0.0575769000
_diffrn_orient_matrix_UB_21      0.0313587000
_diffrn_orient_matrix_UB_22      0.0889114000
_diffrn_orient_matrix_UB_23      0.0146187000
_diffrn_orient_matrix_UB_31      -0.0525028000
_diffrn_orient_matrix_UB_32      0.0472624000
_diffrn_orient_matrix_UB_33      0.0017885000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36746
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.896
_diffrn_reflns_theta_min         3.410
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.766
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       plate
_exptl_crystal_F_000             5020
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         8789
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0392P)^2^+5.9913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6976
_reflns_number_total             8789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00931c1.cif
_cod_data_source_block           acb150018_fa
_cod_database_code               7228513
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C78 H78 Ca2 Cl4 Mn6 N6 O49'
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 O(H,H) groups
2. Restrained distances
 O15-H15B \\sim O15-H15A
 with sigma of 0.02
3. Others
 Fixed Sof: O18(0.25) H18C(0.25) H18D(0.25)
4.a Free rotating group:
 O17(H17A,H17B), O18(H18C,H18D)
4.b Rotating group:
 O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B)
4.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12C,H12D), C18(H18A,H18B)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39)
;
_shelx_res_checksum              98738
_olex2_submission_special_instructions 'No special instructions were received'