Synthesis and Characterization of Calcium Complexes Containing η2-Pyrazolato Ligands
Dirk Pfeiffer; Mary Jane Heeg; Charles H. Winter; Inorganic Chemistry 39 (2000) 2377–2384; doi:10.1021/ic991049c

data_4320971
_publ_section_title
;
 Synthesis and Characterization of Calcium Complexes Containing
 \h2-Pyrazolato Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2377
_journal_page_last               2384
_journal_paper_doi               10.1021/ic991049c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C37 H53 Ca N7'
_chemical_formula_weight         635.94
_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'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 109.6570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3230(4)
_cell_length_b                   15.7572(4)
_cell_length_c                   17.5494(5)
_cell_measurement_reflns_used    5874
_cell_measurement_temperature    295(2)
_cell_volume                     3990.33(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_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  0.064
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_min         1.79
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_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       'elongated octahedron'
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_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0025(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.884
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
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_refine_ls_shift/esd_mean        0.139
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2317
_refine_ls_wR_factor_obs         0.1870
_reflns_number_observed          3638
_reflns_number_total             8413
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991049c_1.cif
_cod_data_source_block           scan(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3990.3(2)
_cod_database_code               4320971