Synthesis of 3- and 5-formyl-4-phenyl-1H-pyrazoles: promising head units for the generation of asymmetric imine ligands and mixed metal polynuclear complexes
Olguín, Juan; Brooker, Sally; New Journal of Chemistry 35 (2011) 1242–; doi:10.1039/c0nj00774a

data_7052638
_publ_section_title
;
 Synthesis of 3- and 5-formyl-4-phenyl-1H-pyrazoles: promising head
 units for the generation of asymmetric imine ligands and mixed metal
 polynuclear complexes
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1242
_journal_paper_doi               10.1039/c0nj00774a
_journal_volume                  35
_journal_year                    2011
_chemical_formula_sum            'C85.75 H72.75 B2 F8 Fe N19.25 Ni3 O2.25'
_chemical_formula_weight         1814.48
_chemical_name_systematic
;
?
;
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.789(7)
_cell_angle_beta                 85.699(7)
_cell_angle_gamma                70.209(6)
_cell_formula_units_Z            2
_cell_length_a                   12.5943(16)
_cell_length_b                   18.395(2)
_cell_length_c                   20.037(3)
_cell_measurement_reflns_used    7792
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      27.403
_cell_measurement_theta_min      2.287
_cell_volume                     4344.9(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
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_diffrn_reflns_theta_max         27.49
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_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.8577
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.40
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     1146
_refine_ls_number_reflns         19810
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_refine_ls_R_factor_all          0.0922
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+12.5899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2040
_reflns_number_gt                16074
_reflns_number_total             19810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00774a.txt
_cod_data_source_block           jo456b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4345.0(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052638