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_7228512
_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         'C36 H36 Ca2 Cl0.8 Mn2 N9.2 O18.8, C3 H6 O'
_chemical_formula_sum            'C39 H42 Ca2 Cl0.8 Mn2 N9.2 O19.8'
_chemical_formula_weight         1174.82
_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     direct
_audit_creation_date             2015-10-29
_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                61.595(6)
_cell_angle_beta                 79.180(5)
_cell_angle_gamma                68.553(5)
_cell_formula_units_Z            1
_cell_length_a                   10.5975(6)
_cell_length_b                   11.4166(7)
_cell_length_c                   11.7527(6)
_cell_measurement_reflns_used    5601
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.7430
_cell_measurement_theta_min      4.2390
_cell_volume                     1163.97(14)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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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 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega -124.00  -78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905 -167.0000  147.0000 46

  2 omega   16.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   38.0000 -180.0000 96

  3 omega  -29.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  -38.0000    0.0000 92

  4 omega   13.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905 -125.0000  -90.0000 39

  5 omega   18.00   71.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000 -168.0853 53

  6 omega   74.00  100.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000 -168.0853 26

  7 omega   84.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  145.1623 37

  8 omega  115.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000   60.0000 61

  9 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -110.6602 26

 10 omega   58.00   83.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  120.0000 25

 11 omega   26.00   61.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -180.0000 35

 12 omega  108.00  134.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   90.0000 26

 13 omega   34.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 41

 14 omega   22.00   61.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  150.0000 39

 15 omega   73.00  124.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  150.0000 51

 16 omega   57.00   90.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000   60.0000 33

 17 omega   19.00   67.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   30.0000 48

 18 omega   73.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  150.0000 85

 19 omega   81.00  147.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  120.0000 66

 20 omega   10.00   41.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  120.0000 31

 21 omega   14.00   74.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -60.0000 60

 22 omega   21.00   70.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000 -150.0000 49

 23 omega   55.00  132.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   52.2936 77

 24 omega   64.00   89.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   90.0000 25

 25 omega   59.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -47.4137 53

 26 omega  144.00  172.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   90.0000 28

 27 omega   54.00   80.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000    0.0000 26

 28 omega    9.00   43.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -47.4137 34

 29 omega  -34.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  -38.0000   90.0000 102

 30 omega    8.00  120.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000 -150.0000 112

 31 omega   12.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   57.0000  -30.0000 104

 32 omega   12.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   57.0000   60.0000 104

 33 omega   63.00  171.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000 -150.0000 108

 34 omega   63.00  168.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  -30.0000 105

 35 omega   63.00  168.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  -90.0000 105

 36 omega   63.00  168.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000   90.0000 105

 37 omega   63.00  168.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000   30.0000 105
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0340105000
_diffrn_orient_matrix_UB_12      0.1230069000
_diffrn_orient_matrix_UB_13      -0.1362529000
_diffrn_orient_matrix_UB_21      -0.1271532000
_diffrn_orient_matrix_UB_22      0.0777159000
_diffrn_orient_matrix_UB_23      0.0554258000
_diffrn_orient_matrix_UB_31      0.0841200000
_diffrn_orient_matrix_UB_32      0.0710382000
_diffrn_orient_matrix_UB_33      0.0240304000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16519
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.007
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.555
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.470
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       plate
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4106
_refine_ls_number_restraints     412
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.7964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3524
_reflns_number_total             4106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00931c1.cif
_cod_data_source_block           acb150020_fa
_cod_original_cell_volume        1163.96(13)
_cod_original_formula_sum        'C39 H42 Ca2 Cl0.80 Mn2 N9.20 O19.80'
_cod_database_code               7228512
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C39 H42 Ca2 Cl1 Mn2 N9 O20'
_reflns_odcompleteness_completeness 99.61
_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 C(H,H,H) groups
2. Restrained distances
 O9-N5 \\sim O8-N5 \\sim O7-N5
 with sigma of 0.02
 Cl1-O11 \\sim Cl1-O12 \\sim Cl1-O13 \\sim Cl1-O10
 with sigma of 0.02
 C21-C20 \\sim C19-C20
 with sigma of 0.02
 O7-O8 \\sim O7-O9 \\sim O8-O9
 with sigma of 0.02
 O10-O11 \\sim O10-O12 \\sim O10-O13 \\sim O11-O12 \\sim O11-O13 \\sim O12-O13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O12) = Uanis(O13)
Uanis(O10) = Uanis(O7)
Uanis(O8) = Uanis(O11)
Uanis(N5) = Uanis(Cl1)
Uanis(O9) = Uanis(O12)
Uanis(C19) = Uanis(C21)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl1(0.40184) O10(0.40184) O11(0.40184) O12(0.40184) O13(0.40184)
 O7(0.59816) O8(0.59816) O9(0.59816) N5(0.59816) O14(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5) C20(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B)
6.b 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)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              77501
_olex2_submission_special_instructions 'No special instructions were received'