Preparation and properties of a calcium(ii)-based molecular chain decorated with manganese(ii) butterfly-like complexes.
Benniston, A. C.; Melnic, S.; Turta, C.; Arauzo, A. B.; Bartolomé, J; Bartolomé, E; Harrington, R. W.; Probert, M. R.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 13349–13357; doi:10.1039/c4dt01518e

data_7031728
_publ_section_title
;
 Preparation and properties of a calcium(ii)-based molecular chain
 decorated with manganese(ii) butterfly-like complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13349
_journal_page_last               13357
_journal_paper_doi               10.1039/c4dt01518e
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C33 H28 Ca2 Cl12 Mn N4 O14'
_chemical_formula_sum            'C33 H28 Ca2 Cl12 Mn N4 O14'
_chemical_formula_weight         1265.09
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.128(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6682(3)
_cell_length_b                   16.9652(4)
_cell_length_c                   17.2318(4)
_cell_measurement_reflns_used    11476
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.5627
_cell_measurement_theta_min      2.8785
_cell_volume                     4869.44(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0419225000
_diffrn_orient_matrix_UB_12      -0.0021687000
_diffrn_orient_matrix_UB_13      -0.0084142000
_diffrn_orient_matrix_UB_21      -0.0003778000
_diffrn_orient_matrix_UB_22      0.0405309000
_diffrn_orient_matrix_UB_23      -0.0101159000
_diffrn_orient_matrix_UB_31      0.0074636000
_diffrn_orient_matrix_UB_32      -0.0100411000
_diffrn_orient_matrix_UB_33      -0.0390294000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28119
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.626
_diffrn_reflns_theta_min         2.884
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       block
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10458
_refine_ls_number_restraints     884
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+12.3388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8476
_reflns_number_total             10458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01518e2.cif
_cod_data_source_block           acb120009
_cod_depositor_comments          'Adding full bibliography for 7031728.cif.'
_cod_database_code               7031728
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.87 with sigma of 0.02
 Cl39-C32A \\sim Cl9-C32 \\sim Cl10-C32 \\sim Cl40-C32A \\sim Cl38-C30A \\sim
Cl8-C30 \\sim Cl37-C30A
 \\sim Cl7-C30 \\sim Cl1-C24A \\sim Cl31-C24 \\sim Cl2-C24A \\sim Cl32-C24
 with sigma of 0.02
 C32A-C31 \\sim C32-C31 \\sim C30A-C29 \\sim C30-C29 \\sim C24A-C23 \\sim
C24-C23
 with sigma of 0.02
 Cl9-Cl10 \\sim Cl39-Cl40 \\sim Cl37-Cl38 \\sim Cl7-Cl8 \\sim Cl1-Cl2 \\sim
Cl31-Cl32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30A) = Uanis(C30)
Uanis(Cl7) = Uanis(Cl37)
Uanis(Cl38) = Uanis(Cl8)
Uanis(Cl1) = Uanis(Cl31)
Uanis(Cl2) = Uanis(Cl32)
Uanis(Cl10) = Uanis(Cl40)
Uanis(Cl39) = Uanis(Cl9)
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
 Sof(Cl1)=Sof(Cl2)=Sof(C24A)=Sof(H24A)=1-FVAR(1)
 Sof(Cl31)=Sof(Cl32)=Sof(C24)=Sof(H24)=FVAR(1)
 Sof(Cl39)=Sof(Cl40)=Sof(C32A)=Sof(H32A)=1-FVAR(2)
 Sof(Cl9)=Sof(Cl10)=Sof(C32)=Sof(H32)=FVAR(2)
 Sof(Cl37)=Sof(Cl38)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(Cl7)=Sof(Cl8)=Sof(C30)=Sof(H30)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C24(H24), C24A(H24A), C26(H26), C27(H27), C30(H30), C30A(H30A), C32(H32),
 C32A(H32A), C34(H34)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20)
6.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C)
;
_shelx_res_checksum              41680