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_7228511
_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         'C40 H42 Ca2 Cl4 Mn2 N8 O18, 2(C3 H6 O)'
_chemical_formula_sum            'C46 H54 Ca2 Cl4 Mn2 N8 O20'
_chemical_formula_weight         1370.81
_chemical_name_systematic
;
 ? 
;
_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   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                90.00
_cell_angle_beta                 107.529(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.660(2)
_cell_length_b                   11.8933(10)
_cell_length_c                   20.3808(14)
_cell_measurement_reflns_used    2508
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      24.7360
_cell_measurement_theta_min      1.7280
_cell_volume                     5699.9(8)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_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   21.00   46.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6314   83.0000   39.0000 25

  2 omega   16.00   86.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6314   38.0000  -90.0000 70

  3 omega  -19.00   14.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.2096  -99.0000  -90.0000 33

  4 omega  -24.00   52.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6314  -99.0000 -180.0000 76

  5 omega  -24.00   22.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.2096  -99.0000   26.0000 46

  6 omega  -79.00  -54.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.2096 -178.0000  -60.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0048702000
_diffrn_orient_matrix_UB_12      0.0485486000
_diffrn_orient_matrix_UB_13      0.0175768000
_diffrn_orient_matrix_UB_21      -0.0281602000
_diffrn_orient_matrix_UB_22      -0.0185675000
_diffrn_orient_matrix_UB_23      -0.0038752000
_diffrn_orient_matrix_UB_31      0.0097302000
_diffrn_orient_matrix_UB_32      -0.0291653000
_diffrn_orient_matrix_UB_33      0.0317463000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.1149
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14020
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.73
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64082
_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.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5019
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.0826
_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^)+(0.0945P)^2^+30.9546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2199
_reflns_number_gt                3317
_reflns_number_total             5019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce00931c1.cif
_cod_data_source_block           shi_2434_sime
_cod_original_cell_volume        5700.0(7)
_cod_database_code               7228511
_chemical_oxdiff_formula         'C30 H40 O8 N4 Mn4 Ca1'
_chemical_oxdiff_usercomment     '0.03 x 0.1 x 0.2 rosu '
_reflns_odcompleteness_completeness 85.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.16
_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) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C23X-C22 \\sim C23-C22 \\sim C23X-C21 \\sim C23-C21
 with sigma of 0.01
 O9-C23X \\sim O9X-C23
 with sigma of 0.01
 Cl1-C20 \\sim Cl1X-C20 \\sim Cl2-C20
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O9) = Uanis(C21) = Uanis(C23X) = Uanis(C22) = Uanis(C23) = Uanis(O9X)
4. Others
 Fixed Sof: H20(0.5) H20A(0.25) H20B(0.25) H21D(0.5) H21E(0.5) H21F(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) H22D(0.5) H22E(0.5) H22F(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) Cl1(0.75) Cl2(0.75) O9X(0.5) C23(0.5) Cl1X(0.5) O9(0.5)
 C23X(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), C20(H20,H20A,H20B), C21(H21D,H21E,H21F), C21(H21A,H21B,H21C),
 C22(H22D,H22E,H22F), C22(H22A,H22B,H22C)
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)
;
_olex2_date_sample_data_collection 2014-03-25
_olex2_submission_special_instructions 'No special instructions were received'