Mixed-metal calix[8]arene complexes: Structure, and ring opening polymerization studies
Xing, Tian; Derbyshire, Max; Elsegood, Mark Robert James; Redshaw, Carl; Chemical Communications  (2022) –; doi:10.1039/D2CC02236B

data_7130201
_publ_section_title
;
 Mixed-metal calix[8]arene complexes: Structure, and ring opening
 polymerization studies
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02236B
_journal_year                    2022
_chemical_formula_moiety         'C92 H110 Mo2 N2 O10, 5(C2 H3 N)'
_chemical_formula_sum            'C102 H125 Mo2 N7 O10'
_chemical_formula_weight         1800.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-06 deposited with the CCDC.	2022-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.2550(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.03282(17)
_cell_length_b                   18.94309(17)
_cell_length_c                   24.7719(2)
_cell_measurement_reflns_used    35706
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2840
_cell_measurement_theta_min      2.9830
_cell_volume                     9644.88(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Buker SHELXTL'
_computing_publication_material  'Buker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
;
Rigaku 007HF equipped with Varimax confocal mirrors and 
an AFC11 goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            87475
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.394
_diffrn_reflns_theta_min         2.507
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.600
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             3800
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1250
_refine_ls_number_reflns         17906
_refine_ls_number_restraints     593
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+9.3056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15405
_reflns_number_total             17906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02236b2.cif
_cod_data_source_block           7dot5MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Iterative' was
changed to 'iterative' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7130201
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              81440
_shelx_hkl_checksum              5225