Probing the structural changes accompanying a spin crossover transition in a chiral [Fe(ii)(N3O2)(CN)2] macrocycle by X-ray crystallography
Acha, Roland T.; Pilkington, Melanie; CrystEngComm 17 (2015) 8897–; doi:10.1039/C5CE01052G

data_7221051
_publ_section_title
;
 Probing the structural changes accompanying a spin crossover transition
 in a chiral [Fe(ii)(N3O2)(CN)2] macrocycle by X-ray crystallography
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8897
_journal_paper_doi               10.1039/C5CE01052G
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C33 H37 Fe N5 O4, H2 O'
_chemical_formula_sum            'C33 H39 Fe N5 O5'
_chemical_formula_weight         641.54
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-05-29 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                76.045(3)
_cell_angle_beta                 80.991(2)
_cell_angle_gamma                71.463(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5843(6)
_cell_length_b                   10.6128(10)
_cell_length_c                   21.007(2)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.80
_cell_measurement_theta_min      2.48
_cell_volume                     1549.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0417
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33992
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.846
_diffrn_reflns_theta_min         2.005
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       needle
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 4824 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.171(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         16024
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+2.2270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.714
_reflns_friedel_fraction_full    0.884
_reflns_friedel_fraction_max     0.684
_reflns_number_gt                12982
_reflns_number_total             16024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01052g2.cif
_cod_data_source_block           fulldat
_cod_depositor_comments
'Adding full bibliography for 7221050--7221051.cif.'
_cod_database_code               7221051
_shelxl_version_number           2014-3
_shelx_res_checksum              2132