Tuning of crystallization method and ligand conformation to give a mononuclear compound or two-dimensional SCO coordination polymer based on a new semi-rigid V-shaped bis-pyridyl bis-amide ligand
Hao, Xiaoyun; Dou, Yong; Cao, Tong; Qin, Lan; Yang, Lu; Liu, Hui; Li, Dacheng; Liu, Qingyun; Zhang, Daopeng; Zhou, Zhen; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620004854

data_2022086
_publ_section_title
;
 Tuning of crystallization method and ligand conformation to give a
 mononuclear compound or two-dimensional SCO coordination polymer based on
 a new semi-rigid V-shaped bis-pyridyl bis-amide ligand
;
_journal_coeditor_code           LF3116
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620004854
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Fe (S C N)2 (C19 H16 N4 O2)2 (C H4 O)2]'
_chemical_formula_moiety         'C42 H40 Fe N10 O6 S2'
_chemical_formula_sum            'C42 H40 Fe N10 O6 S2'
_chemical_formula_weight         900.81
_chemical_name_systematic
Bis(methanol-\k<i>O</i>)bis[5-methyl-<i>N</i>,<i>N</i>'-bis(pyridin-4-yl)benzene-1,3-dicarboxamide-\k<i>N</i>]bis(thiocyanato-\k<i>N</i>)iron(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                82.848(7)
_cell_angle_beta                 84.322(7)
_cell_angle_gamma                67.522(8)
_cell_formula_units_Z            1
_cell_length_a                   9.0061(7)
_cell_length_b                   10.3811(8)
_cell_length_c                   11.6830(9)
_cell_measurement_reflns_used    2433
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8735
_cell_measurement_theta_min      2.9308
_cell_volume                     999.87(15)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2001)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2001)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6227
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.937
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3530
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0511P)^2^+0.4901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                2889
_reflns_number_total             3530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3116sup1.cif
_cod_data_source_block           mono
_cod_database_code               2022086
_cod_database_fobs_code          2022086
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.953
_shelx_hkl_checksum              92248
_shelx_res_checksum              8333