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_7228510
_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         'C25 H24 Ca Cl Mn N3 O6, Cl O3.95'
_chemical_formula_sum            'C25 H24 Ca Cl2 Mn N3 O9.95'
_chemical_formula_weight         691.59
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-05-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                87.205(4)
_cell_angle_beta                 89.130(4)
_cell_angle_gamma                88.881(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4621(5)
_cell_length_b                   11.6521(5)
_cell_length_c                   12.3464(5)
_cell_measurement_reflns_used    4522
_cell_measurement_temperature    172.95(10)
_cell_measurement_theta_max      28.3030
_cell_measurement_theta_min      1.7550
_cell_volume                     1502.86(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   10.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6314   57.0000 -150.0000 59

  2 omega   55.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6314  178.0000    0.0000 35

  3 omega  -25.00   20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.2096  -99.0000  120.0000 45

  4 omega  -81.00  -36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.2096 -178.0000 -120.0000 45

  5 omega   42.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6314 -178.0000  150.0000 46

  6 omega  -23.00   12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.2877  -99.0000  -30.0000 35

  7 omega   -3.00   34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7877  -38.0000  150.0000 37

  8 omega  -49.00  -23.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7877  -38.0000  150.0000 26

  9 omega  -38.00   13.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7877  -77.0000  -60.0000 51

 10 omega    3.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7877   38.0000  120.0000 83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0099336000
_diffrn_orient_matrix_UB_12      0.0395725000
_diffrn_orient_matrix_UB_13      -0.0447044000
_diffrn_orient_matrix_UB_21      0.0549887000
_diffrn_orient_matrix_UB_22      0.0302748000
_diffrn_orient_matrix_UB_23      0.0141882000
_diffrn_orient_matrix_UB_31      0.0384279000
_diffrn_orient_matrix_UB_32      -0.0351156000
_diffrn_orient_matrix_UB_33      -0.0333051000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0549
_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       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12990
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             707
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+2.9314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1556
_reflns_number_gt                4394
_reflns_number_total             5302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce00931c1.cif
_cod_data_source_block           shi_2435_sime
_cod_original_cell_volume        1502.87(12)
_cod_database_code               7228510
_chemical_oxdiff_formula         'C30 H40 N2 O8 Mn1 Ca1 Cl2'
_chemical_oxdiff_usercomment     OEC_16
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 Cl2-O8 \\sim Cl2-O9X \\sim Cl2-O8X \\sim Cl2-O7X \\sim Cl2-O7 \\sim Cl2-O9
\\sim Cl2-O6X \\sim Cl2-O6
 with sigma of 0.01
 Cl3-O11 \\sim Cl3-O12X \\sim Cl3-O11X \\sim Cl3-O14X \\sim Cl3-O10 \\sim
Cl3-O13X \\sim Cl3-O12 \\sim Cl3-
 O13
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(O7X) = Uiso(O6) = Uiso(O8) = Uiso(O9) = Uiso(O6X) = Uiso(O7) = Uiso(O8X) =
Uiso(O9X)
Uiso(O11) = Uiso(O10) = Uiso(O14X) = Uiso(O13) = Uiso(O13X) = Uiso(O12) =
Uiso(O12X) = Uiso(O11X) = Uiso(O10X)
4. Others
 Fixed Sof: O10X(0.2) O11X(0.25) Cl3(0.5) O10(0.2) O11(0.2) O12(0.25)
 O12X(0.2) O13(0.2) O13X(0.25) O14X(0.2) O9X(0.25) Cl2(0.5) O6(0.25) O6X(0.25)
 O7(0.25) O7X(0.25) O8(0.25) O9(0.25) O8X(0.25)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C25(H25)
;
_olex2_date_sample_data_collection 2014-03-25
_olex2_submission_special_instructions 'No special instructions were received'