Calcium and heterometallic manganese-calcium complexes supported by tripodal pyridine-carboxylate ligands: structural, EPR and theoretical investigations.
Gerey, Bertrand; Gennari, Marcello; Gouré, Eric; Pécaut, Jacques; Blackman, Allan; Pantazis, Dimitrios A.; Neese, Frank; Molton, Florian; Fortage, Jérôme; Duboc, Carole; Collomb, Marie-Noëlle; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12757–12770; doi:10.1039/c5dt01776a

data_7035379
_publ_section_title
;
 Calcium and heterometallic manganese-calcium complexes supported by
 tripodal pyridine-carboxylate ligands: structural, EPR and theoretical
 investigations.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12757
_journal_page_last               12770
_journal_paper_doi               10.1039/c5dt01776a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C24 H39 Ca Cl2 Mn N4 O11.5'
_chemical_formula_weight         733.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-04-07 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.324(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7202(2)
_cell_length_b                   14.6163(3)
_cell_length_c                   13.0992(3)
_cell_measurement_reflns_used    4093
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4143
_cell_measurement_theta_min      3.4065
_cell_volume                     1666.78(6)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   44.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  179.0000 -180.0000 27

  2 omega   40.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  179.0000  -90.0000 26

  3 omega  -18.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   57.0000  150.0000 60

  4 omega  -53.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   37.0000  -60.0000 97

  5 omega  -97.00  -48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000 -180.0000 49

  6 omega    6.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   60.0000   22.0000 88

  7 omega    1.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000  -60.0000 32

  8 omega   61.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000  -60.0000 35

  9 omega -100.00  -65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -37.0000  120.0000 35

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18389
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_correction_T_min  0.7929
_exptl_absorpt_correction_type   analytical
_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)
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            'light yellow'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         10046
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                8219
_reflns_number_total             10046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01776a2.cif
_cod_data_source_block           '[Mn(tpada)ClCa(OH2)3(MeOH)2]Cl'
_cod_depositor_comments
'Adding full bibliography for 7035379--7035380.cif.'
_cod_original_cell_volume        1666.79(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C24 H39 Ca Cl2 Mn N4 O11.50'
_cod_database_code               7035379