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_7221050
_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, (O)'
_chemical_formula_sum            'C33 H37 Fe N5 O5'
_chemical_formula_weight         639.53
_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   geom
_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                76.939(6)
_cell_angle_beta                 80.725(6)
_cell_angle_gamma                72.021(6)
_cell_formula_units_Z            2
_cell_length_a                   7.6279(9)
_cell_length_b                   10.6208(13)
_cell_length_c                   20.927(3)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      30.77
_cell_measurement_theta_min      2.45
_cell_volume                     1563.2(4)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24813
_diffrn_reflns_point_group_measured_fraction_full 0.782
_diffrn_reflns_point_group_measured_fraction_max 0.757
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.008
_exptl_absorpt_coefficient_mu    0.532
_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    1.363
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 2718 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.241(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         10321
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+4.6982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2142
_reflns_Friedel_coverage         0.533
_reflns_friedel_fraction_full    0.573
_reflns_friedel_fraction_max     0.526
_reflns_number_gt                8957
_reflns_number_total             10321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01052g2.cif
_cod_data_source_block           rolandmay102011_0m
_cod_depositor_comments
'Adding full bibliography for 7221050--7221051.cif.'
_cod_original_cell_volume        1563.2(3)
_cod_database_code               7221050
_shelxl_version_number           2014-3
_shelx_res_checksum              32967