Self-assembly of thiolato-bridged ester-functionalized Re(i)-based tetranuclear spiro-metallacyclophanes
Varghese, Jisna; Kumar, Udit; Jose, Shilpa; Magray, Aamir Afzal; Yeswanth Kumar, S.; Padmanaban, R.; Manimaran, Bala.; New Journal of Chemistry 47 (2023) 3582–3590; doi:10.1039/D2NJ04784E

data_7062256
_publ_section_title
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 Self-assembly of thiolato-bridged ester-functionalized Re(i)-based
 tetranuclear spiro-metallacyclophanes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3582
_journal_page_last               3590
_journal_paper_doi               10.1039/D2NJ04784E
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'C69 H52 N4 O20 Re4 S4, 2(C H3 N O2), C H2 Cl2, 1[CH2Cl2]'
_chemical_formula_sum            'C72 H60 Cl2 N6 O24 Re4 S4'
_chemical_formula_weight         2337.301
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_audit_creation_date             2022-11-16
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.10.29 svn.ra8b101fa for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-12-05 deposited with the CCDC.	2023-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.264(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.379(4)
_cell_length_b                   21.639(3)
_cell_length_c                   17.878(3)
_cell_measurement_reflns_used    9729
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.45
_cell_volume                     8332(2)
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.9981
_diffrn_reflns_Laue_measured_fraction_max 0.9982
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57529
_diffrn_reflns_point_group_measured_fraction_full 0.9981
_diffrn_reflns_point_group_measured_fraction_max 0.9982
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    6.032
_exptl_absorpt_correction_T_max  0.0151
_exptl_absorpt_correction_T_min  0.0012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1520 before and 0.0998 after correction.
The Ratio of minimum to maximum transmission is 0.0795.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4492.894
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.5326
_refine_diff_density_min         -1.1082
_refine_diff_density_rms         0.2303
_refine_ls_d_res_high            0.8001
_refine_ls_d_res_low             8.8887
_refine_ls_goodness_of_fit_ref   1.0551
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    55
_refine_ls_number_parameters     557
_refine_ls_number_reflns         8510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0551
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+86.7105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1394
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -32
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7251
_reflns_number_total             8510
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj04784e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7062256.cif.'
_cod_database_code               7062256
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H2Wa(0.5) H2Wb(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b), C1(H1a,H1b), C8(H8a,H8b), C23(H23a,H23b), C2W(H2Wa,H2Wb)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C18(H18), C29(H29), C19(H19), C28(H28), C27(H27), C3(H3),
 C26(H26), C7(H7), C14(H14), C12(H12), C13(H13), C4(H4), C10(H10), C5(H5),
 C11(H11), C6(H6)
4.c Idealised Me refined as rotating group:
 C0AA(H0Aa,H0Ab,H0Ac)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 164 electrons were 
found in a volume of 810\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1[CH2Cl2] per Formula Unit 
which account for 168 electrons per unit cell.
;
_olex2_submission_special_instructions 'No special instructions were received'