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_7035380
_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            'C40 H50.4 Ca2 N8 O17.2'
_chemical_formula_weight         998.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_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                 113.840(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1802(5)
_cell_length_b                   23.6482(6)
_cell_length_c                   10.2620(4)
_cell_measurement_reflns_used    2661
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3784
_cell_measurement_theta_min      3.3682
_cell_volume                     2259.72(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_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega    7.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   57.0000  120.0000 79

  2 omega  -17.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   19.0000  -90.0000 26

  3 omega   64.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   19.0000  -90.0000 28

  4 omega  -43.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -68.0000  -35.0000 81

  5 omega  -47.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -19.0000   90.0000 25

;
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11187
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.9641
_exptl_absorpt_correction_T_min  0.8551
_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            colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5512
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.4458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                4033
_reflns_number_total             5512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01776a2.cif
_cod_data_source_block           '[Ca(tpada)(OH2)2]2'
_cod_depositor_comments
'Adding full bibliography for 7035379--7035380.cif.'
_cod_original_cell_volume        2259.69(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C40 H50.40 Ca2 N8 O17.20'
_cod_database_code               7035380