Spin-crossover in iron(ii) coordination compounds with 2,6-bis(benzimidazol-2-yl)pyridine
Ivanova, A. D.; Korotaev, E. V.; Komarov, V. Yu.; Sheludyakova, L. A.; Varnek, V. A.; Lavrenova, L. G.; New Journal of Chemistry 44 (2020) 5834–5840; doi:10.1039/D0NJ00474J

data_7059401
_publ_section_title
;
 Spin-crossover in iron(ii) coordination compounds with
 2,6-bis(benzimidazol-2-yl)pyridine
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5834
_journal_page_last               5840
_journal_paper_doi               10.1039/D0NJ00474J
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'2(Br -1), Ni 2(C19 H13 N5) +2, 1.23(H2 O), 3.33(C2 H6 O)'
_chemical_formula_sum            'C44.66 H48.45 Br2 N10 Ni O4.56'
_chemical_formula_weight         1016.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-12 deposited with the CCDC.	2020-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2852(7)
_cell_length_b                   24.0027(8)
_cell_length_c                   19.1159(6)
_cell_measurement_reflns_used    9489
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.23
_cell_volume                     9303.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.751
_diffrn_reflns_theta_min         1.675
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.189
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0695 before and 0.0428 after correction. The Ratio of minimum to maximum transmission is 0.7312. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour
;
 pleochroic brownish green to reddish orange 
;
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             4167
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.382
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1119
_refine_ls_number_reflns         17751
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0849P)^2^+4.1268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10956
_reflns_number_total             17751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00474j1.cif
_cod_data_source_block           llg055_150k_fresh
_cod_depositor_comments
;Adding full bibliography for 7059401.cif.

 Adding full bibliography for 7059401.cif.
;
_cod_database_code               7059401
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.431
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C61S-O6S = C71S-O7S = C81S-O8S = C91S-O9S
 1.45 with sigma of 0.005
 C62S-C61S = C72S-C71S = C82S-C81S = C92S-C91S
 1.5 with sigma of 0.005
 O6S-C62S = O7S-C72S = C82S-O8S = C92S-O9S
 2.36 with sigma of 0.02
3. Rigid bond restraints
 O1S, C11S, C12S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3S, C31S, C32S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uiso(C72S) = Uiso(C62S)
Uiso(C61S) = Uiso(C71S)
Uiso(O6S) = Uiso(O7S)
Uiso(O8S) = Uiso(O9S)
Uiso(C81S) = Uiso(C91S)
Uiso(C82S) = Uiso(C92S)
5. Others
 Sof(O6S)=Sof(H6S)=Sof(C61S)=Sof(H61A)=Sof(H61B)=Sof(C62S)=Sof(H62A)=Sof(H62B)=
 Sof(H62C)=FVAR(1)
 Sof(O7S)=Sof(H7S)=Sof(C71S)=Sof(H71A)=Sof(H71B)=Sof(C72S)=Sof(H72A)=Sof(H72B)=
 Sof(H72C)=FVAR(2)
 Sof(O8S)=Sof(H8S)=Sof(C81S)=Sof(H81A)=Sof(H81B)=Sof(C82S)=Sof(H82A)=Sof(H82B)=
 Sof(H82C)=FVAR(3)
 Sof(O9S)=Sof(H9S)=Sof(C91S)=Sof(H91A)=Sof(H91B)=Sof(C92S)=Sof(H92A)=Sof(H92B)=
 Sof(H92C)=FVAR(4)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(5)
 Sof(O2W)=Sof(H2WA)=Sof(H2WB)=FVAR(6)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O1S(H1S), O2S(H2S), O3S(H3S),
 O4S(H4S), O5S(H5S), O6S(H6S), O7S(H7S), O8S(H8S), O9S(H9S)
6.b Secondary CH2 refined with riding coordinates:
 C11S(H11A,H11B), C21S(H21A,H21B), C31S(H31A,H31B), C41S(H41A,H41B), C51S(H51A,
 H51B), C61S(H61A,H61B), C71S(H71A,H71B), C81S(H81A,H81B), C91S(H91A,H91B)
6.c Aromatic/amide H refined with riding coordinates:
 N129(H129), N139(H139), N159(H159), N169(H169), C113(H113), C114(H114),
 C115(H115), C124(H124), C125(H125), C126(H126), C127(H127), C134(H134),
 C135(H135), C136(H136), C137(H137), C143(H143), C144(H144), C145(H145),
 C154(H154), C155(H155), C156(H156), C157(H157), C164(H164), C165(H165),
 C166(H166), C167(H167), N229(H229), N239(H239), N259(H259), N269(H269),
 C213(H213), C214(H214), C215(H215), C224(H224), C225(H225), C226(H226),
 C227(H227), C234(H234), C235(H235), C236(H236), C237(H237), C243(H243),
 C244(H244), C245(H245), C254(H254), C255(H255), C256(H256), C257(H257),
 C264(H264), C265(H265), C266(H266), C267(H267)
6.d Idealised Me refined with riding coordinates:
 C12S(H12A,H12B,H12C), C22S(H22A,H22B,H22C), C32S(H32A,H32B,H32C), C42S(H42A,
 H42B,H42C), C52S(H52A,H52B,H52C), C62S(H62A,H62B,H62C), C72S(H72A,H72B,H72C),
 C82S(H82A,H82B,H82C), C92S(H92A,H92B,H92C)
;
_shelx_res_checksum              92350
_olex2_submission_special_instructions 'No special instructions were received'