Preparation of dihydroquinazoline carbohydrazone Fe(ii) complexes for spin crossover
Shen, Fu-Xing; Huang, Wei; Yamamoto, Takashi; Einaga, Yasuaki; Wu, Dayu; New J. Chem. 40 (2016) 4534–; doi:10.1039/C5NJ03095A

data_7055395
_publ_section_title
;
 Preparation of dihydroquinazoline carbohydrazone Fe(ii) complexes for
 spin crossover
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              4534
_journal_paper_doi               10.1039/C5NJ03095A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C42 H34 Fe N8 O4, 2(Cl O4)'
_chemical_formula_sum            'C42 H34 Cl2 Fe N8 O12'
_chemical_formula_weight         969.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-20 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.579(10)
_cell_length_b                   17.101(4)
_cell_length_c                   18.604(4)
_cell_measurement_reflns_used    1406
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.70
_cell_measurement_theta_min      2.48
_cell_volume                     10365(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16152
_diffrn_reflns_point_group_measured_fraction_full 0.796
_diffrn_reflns_point_group_measured_fraction_max 0.760
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.674
_diffrn_reflns_theta_min         1.734
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 509 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4609
_refine_ls_number_restraints     410
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.2022
_refine_ls_R_factor_gt           0.0958
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1740P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2304
_refine_ls_wR_factor_ref         0.3048
_reflns_Friedel_coverage         0.498
_reflns_Friedel_fraction_full    0.578
_reflns_Friedel_fraction_max     0.521
_reflns_number_gt                1951
_reflns_number_total             4609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03095a1.cif
_cod_data_source_block           5-296K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055389--7055395.cif.
;
_cod_database_code               7055395
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              66475