Ca K-Edge XAS as a Probe of Calcium Centers in Complex Systems.
Martin-Diaconescu, Vlad; Gennari, Marcello; Gerey, Bertrand; Tsui, Emily; Kanady, Jacob; Tran, Rosalie; Pécaut, Jacques; Maganas, Dimitrios; Krewald, Vera; Gouré, Eric; Duboc, Carole; Yano, Junko; Agapie, Theodor; Collomb, Marie-Noelle; DeBeer, Serena; Inorganic chemistry 54 (2015) 1283–1292; doi:10.1021/ic501991e

data_4341933
_publ_section_title
;
 Ca K-Edge XAS as a Probe of Calcium Centers in Complex Systems.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1283
_journal_page_last               1292
_journal_paper_doi               10.1021/ic501991e
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C22 H34 Ca2 N2 O14'
_chemical_formula_weight         630.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.118(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.8494(6)
_cell_length_b                   9.8491(4)
_cell_length_c                   8.3210(4)
_cell_measurement_reflns_used    1851
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2355
_cell_measurement_theta_min      3.3883
_cell_volume                     1379.94(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   -3.00   93.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000   90.0000 96

  2 omega   34.00   60.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000   60.0000 26

  3 omega  -56.00   41.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801   77.0000    0.0000 97

;
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6154
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.8982
_exptl_absorpt_correction_T_min  0.6739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long bloc'
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0336P)^2^+0.0813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                2839
_reflns_number_total             3395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501991e_si_002.cif
_cod_data_source_block           '[Ca2(bzida)2(H2O)6]n_8i'
_cod_depositor_comments          'Adding full bibliography for 4341933.cif.'
_cod_original_cell_volume        1379.93(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4341933